Benzoxazine resin and their nanostructured composites cure kinetic by DSC

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Obtenção e caracterização térmica de compósitos nanoestruturados de resina fenol-furfurílica/CNT

Pós-graduação em Engenharia Mecânica - FEG

Characterization of thermal and mechanical properties of polypropylene-based composites for fuel cell bipolar plates and development of educational tools in hydrogen and fuel cell technologies

In this project we developed conductive thermoplastic resins by adding varying amounts of three different carbon fillers: carbon black (CB), synthetic graphite (SG) and multi-walled carbon nanotubes (CNT) to a polypropylene matrix for application as fuel cell bipolar plates. This component of fuel cells provides mechanical support to the stack, circulates the gases that participate in the electrochemical reaction within the fuel cell and allows for removal of the excess heat from the system. The materials fabricated in this work were tested to determine their mechanical and thermal properties. These materials were produced by adding varying amounts of single carbon fillers to a polypropylene matrix (2.5 to 15 wt.% Ketjenblack EC-600 JD carbon black, 10 to 80 wt.% Asbury Carbon's Thermocarb TC-300 synthetic graphite, and 2.5 to 15 wt.% of Hyperion Catalysis International's FIBRILTM multi-walled carbon nanotubes) In addition, composite materials containing combinations of these three fillers were produced. The thermal conductivity results showed an increase in both through-plane and in-plane thermal conductivities, with the largest increase observed for synthetic graphite. The Department of Energy (DOE) had previously set a thermal conductivity goal of 20 W/m·K, which was surpassed by formulations containing 75 wt.% and 80 wt.% SG, yielding in-plane thermal conductivity values of 24.4 W/m·K and 33.6 W/m·K, respectively. In addition, composites containing 2.5 wt.% CB, 65 wt.% SG, and 6 wt.% CNT in PP had an in–plane thermal conductivity of 37 W/m·K. Flexural and tensile tests were conducted. All composite formulations exceeded the flexural strength target of 25 MPa set by DOE. The tensile and flexural modulus of the composites increased with higher concentration of carbon fillers. Carbon black and synthetic graphite caused a decrease in the tensile and flexural strengths of the composites. However, carbon nanotubes increased the composite tensile and flexural strengths. Mathematical models were applied to estimate through-plane and in-plane thermal conductivities of single and multiple filler formulations, and tensile modulus of single-filler formulations. For thermal conductivity, Nielsen's model yielded accurate thermal conductivity values when compared to experimental results obtained through the Flash method. For prediction of tensile modulus Nielsen's model yielded the smallest error between the predicted and experimental values. The second part of this project consisted of the development of a curriculum in Fuel Cell and Hydrogen Technologies to address different educational barriers identified by the Department of Energy. By the creation of new courses and enterprise programs in the areas of fuel cells and the use of hydrogen as an energy carrier, we introduced engineering students to the new technologies, policies and challenges present with this alternative energy. Feedback provided by students participating in these courses and enterprise programs indicate positive acceptance of the different educational tools. Results obtained from a survey applied to students after participating in these courses showed an increase in the knowledge and awareness of energy fundamentals, which indicates the modules developed in this project are effective in introducing students to alternative energy sources.

Enhancing the thermomechanical behaviour of poly(phenylene sulphide) based composites via incorporation of covalently grafted carbon nanotubes

The thermal and thermomechanical properties of poly(phenylene sulphide) (PPS) based nanocomposites incorporating a polymer derivative covalently anchored onto single-walled carbon nanotubes (SWCNTs) were investigated. The grafted fillers acted as nucleating agents, increasing the crystallization temperature and degree of crystallinity of the matrix. They also enhanced its thermal stability, flame retardancy, glass transition (Tg) and heat deflection temperatures while reduced the coefficient of thermal expansion at temperatures below Tg. A strong rise in the thermal conductivity, Young?s modulus and tensile strength was found with increasing filler loading both in the glassy and rubbery states. All these outstanding improvements are ascribed to strong matrix-filler interfacial interactions combined with a compatibilization effect that results in very homogeneous SWCNT dispersion. The results herein offer useful insights towards the development of engineering thermoplastic/CNT nanocomposites for high-temperature applications.

Polymer interaction with macroscopic carbon nanotube fibres and fabrication of nanostructured composites

El ensamblado de nanotubos de carbono (CNT) como una fibra macroscópica en la cual están orientados preferentemente paralelos entre sí y al eje de la fibra, ha dado como resultado un nuevo tipo de fibra de altas prestaciones derivadas de la explotación eficiente de las propiedades axiales de los CNTs, y que tiene un gran número de aplicaciones potenciales. Fibras continuas de CNTs se produjeron en el Instituto IMDEA Materiales mediante el proceso de hilado directo durante la reacción de síntesis por deposición química de vapores. Uno de los objetivos de esta tesis es el estudio de la estructura de estas fibras mediante técnicas del estado del arte de difracción de rayos X de sincrotrón y la elaboración de un modelo estructural de dicho material. Mediciones texturales de adsorción de gases, análisis de micrografías de electrones y dispersión de rayos X de ángulo alto y bajo (WAXS/SAXS) indican que el material tiene una estructura mesoporosa con una distribución de tamaño de poros ancha derivada del amplio rango de separaciones entre manojos de CNTs, así como una superficie específica de 170m2/g. Los valores de dimensión fractal obtenidos mediante SAXS y análisis Barrett-Joyner-Halenda (BJH) de mediciones texturales coinciden en 2.4 y 2.5, respectivamente, resaltando el carácter de red de la estructura de dichas fibras. La estructura mesoporosa y tipo hilo de las fibra de CNT es accesible a la infiltración de moléculas externas (líquidos o polímeros). En este trabajo se estudian los cambios en la estructura multiescala de las fibras de CNTs al interactuar con líquidos y polímeros. Los efectos de la densificación en la estructura de fibras secas de CNT son estudiados mediante WAXS/SAXS. El tratamiento de densificación junta los manojos de la fibra (los poros disminuyen de tamaño), resultando en un incremento de la densidad de la fibra. Sin embargo, los dominios estructurales correspondientes a la transferencia de esfuerzo mecánica y carga eléctrica en los nanotubos no son afectados durante este proceso de densificación; como consecuencia no se produce un efecto sustancial en las propiedades mecánicas y eléctricas. Mediciones de SAXS and fibra de CNT antes y después de infiltración de líquidos confirman la penetración de una gran cantidad de líquidos que llena los poros internos de la fibra pero no se intercalan entre capas de nanotubos adyacentes. La infiltración de cadenas poliméricas de bajo peso molecular tiende a expandir los manojos en la fibra e incrementar el ángulo de apertura de los poros. Los resultados de SAXS indican que la estructura interna de la fibra en términos de la organización de las capas de tubos y su orientación no es afectada cuando las muestras consisten en fibras infiltradas con polímeros de alto peso molecular. La cristalización de varios polímeros semicristalinos es acelerada por la presencia de fibras de CNTs alineados y produce el crecimiento de una capa transcristalina normal a la superficie de la fibra. Esto es observado directamente mediante microscopía óptica polarizada, y detectado mediante calorimetría DSC. Las lamelas en la capa transcristalina tienen orientación de la cadena polimérica paralela a la fibra y por lo tanto a los nanotubos, de acuerdo con los patrones de WAXS. Esta orientación preferencial se sugiere como parte de la fuerza impulsora en la nucleación. La nucleación del dominio cristalino polimérico en la superficie de los CNT no es epitaxial. Ocurre sin haber correspondencia entre las estructuras cristalinas del polímero y los nanotubos. Estas observaciones contribuyen a la compresión del fenómeno de nucleación en CNTs y otros nanocarbonos, y sientan las bases para el desarrollo de composites poliméricos de gran escala basados en fibra larga de CNTs alineados. ABSTRACT The assembly of carbon nanotubes into a macroscopic fibre material where they are preferentially aligned parallel to each other and to the fibre axis has resulted in a new class of high-performance fibres, which efficiently exploits the axial properties of the building blocks and has numerous applications. Long, continuous CNT fibres were produced in IMDEA Materials Institute by direct fibre spinning from a chemical vapour deposition reaction. These fibres have a complex hierarchical structure covering multiple length scales. One objective of this thesis is to reveal this structure by means of state-of-the-art techniques such as synchrotron X-ray diffraction, and to build a model to link the fibre structural elements. Texture and gas absorption measurements, using electron microscopy, wide angle and small angle X-ray scattering (WAXS/SAXS), and pore size distribution analysis by Barrett-Joyner-Halenda (BJH), indicate that the material has a mesoporous structure with a wide pore size distribution arising from the range of fibre bundle separation, and a high surface area _170m2/g. Fractal dimension values of 2.4_2.5 obtained from the SAXS and BJH measurements highlight the network structure of the fibre. Mesoporous and yarn-like structure of CNT fibres make them accessible to the infiltration of foreign molecules (liquid or polymer). This work studies multiscale structural changes when CNT fibres interact with liquids and polymers. The effects of densification on the structure of dry CNT fibres were measured by WAXS/SAXS. The densification treatment brings the fibre bundles closer (pores become smaller), leading to an increase in fibre density. However, structural domains made of the load and charge carrying nanotubes are not affected; consequently, it has no substantial effect on mechanical and electrical properties. SAXS measurements on the CNT fibres before and after liquid infiltration imply that most liquids are able to fill the internal pores but not to intercalate between nanotubes. Successful infiltration of low molecular weight polymer chains tends to expand the fibre bundles and increases the pore-opening angle. SAXS results indicate that the inner structure of the fibre, in terms of the nanotube layer arrangement and the fibre alignment, are not largely affected when infiltrated with polymers of relatively high molecular weight. The crystallisation of a variety of semicrystalline polymers is accelerated by the presence of aligned fibres of CNTs and results in the growth of a transcrystalline layer perpendicular to the fibre surface. This can be observed directly under polarised optical microscope, and detected by the exothermic peaks during differential scanning calorimetry. The discussion on the driving forces for the enhanced nucleation points out the preferential chain orientation of polymer lamella with the chain axis parallel to the fibre and thus to the nanotubes, which is confirmed by two-dimensional WAXS patterns. A non-epitaxial polymer crystal growth habit at the CNT-polymer interface is proposed, which is independent of lattice matching between the polymer and nanotubes. These findings contribute to the discussion on polymer nucleation on CNTs and other nanocarbons, and their implication for the development of large polymer composites based on long and aligned fibres of CNTs.

Plasma and cold sprayed aluminum carbon nanotube composites: Quantification of nanotube distribution and multi-scale mechanical properties

Carbon nanotubes (CNT) could serve as potential reinforcement for metal matrix composites for improved mechanical properties. However dispersion of carbon nanotubes (CNT) in the matrix has been a longstanding problem, since they tend to form clusters to minimize their surface area. The aim of this study was to use plasma and cold spraying techniques to synthesize CNT reinforced aluminum composite with improved dispersion and to quantify the degree of CNT dispersion as it influences the mechanical properties. Novel method of spray drying was used to disperse CNTs in Al-12 wt.% Si prealloyed powder, which was used as feedstock for plasma and cold spraying. A new method for quantification of CNT distribution was developed. Two parameters for CNT dispersion quantification, namely Dispersion parameter (DP) and Clustering Parameter (CP) have been proposed based on the image analysis and distance between the centers of CNTs. Nanomechanical properties were correlated with the dispersion of CNTs in the microstructure. Coating microstructure evolution has been discussed in terms of splat formation, deformation and damage of CNTs and CNT/matrix interface. Effect of Si and CNT content on the reaction at CNT/matrix interface was thermodynamically and kinetically studied. A pseudo phase diagram was computed which predicts the interfacial carbide for reaction between CNT and Al-Si alloy at processing temperature. Kinetic aspects showed that Al4C3 forms with Al-12 wt.% Si alloy while SiC forms with Al-23wt.% Si alloy. Mechanical properties at nano, micro and macro-scale were evaluated using nanoindentation and nanoscratch, microindentation and bulk tensile testing respectively. Nano and micro-scale mechanical properties (elastic modulus, hardness and yield strength) displayed improvement whereas macro-scale mechanical properties were poor. The inversion of the mechanical properties at different scale length was attributed to the porosity, CNT clustering, CNT-splat adhesion and Al 4C3 formation at the CNT/matrix interface. The Dispersion parameter (DP) was more sensitive than Clustering parameter (CP) in measuring degree of CNT distribution in the matrix.

Plasma And Cold Sprayed Aluminum Carbon Nanotube Composites: Quantification Of Nanotube Distribution And Multi-Scale Mechanical Properties

Carbon nanotubes (CNT) could serve as potential reinforcement for metal matrix composites for improved mechanical properties. However dispersion of carbon nanotubes (CNT) in the matrix has been a longstanding problem, since they tend to form clusters to minimize their surface area. The aim of this study was to use plasma and cold spraying techniques to synthesize CNT reinforced aluminum composite with improved dispersion and to quantify the degree of CNT dispersion as it influences the mechanical properties. Novel method of spray drying was used to disperse CNTs in Al-12 wt.% Si pre-alloyed powder, which was used as feedstock for plasma and cold spraying. A new method for quantification of CNT distribution was developed. Two parameters for CNT dispersion quantification, namely Dispersion parameter (DP) and Clustering Parameter (CP) have been proposed based on the image analysis and distance between the centers of CNTs. Nanomechanical properties were correlated with the dispersion of CNTs in the microstructure. Coating microstructure evolution has been discussed in terms of splat formation, deformation and damage of CNTs and CNT/matrix interface. Effect of Si and CNT content on the reaction at CNT/matrix interface was thermodynamically and kinetically studied. A pseudo phase diagram was computed which predicts the interfacial carbide for reaction between CNT and Al-Si alloy at processing temperature. Kinetic aspects showed that Al4C3 forms with Al-12 wt.% Si alloy while SiC forms with Al-23wt.% Si alloy. Mechanical properties at nano, micro and macro-scale were evaluated using nanoindentation and nanoscratch, microindentation and bulk tensile testing respectively. Nano and micro-scale mechanical properties (elastic modulus, hardness and yield strength) displayed improvement whereas macro-scale mechanical properties were poor. The inversion of the mechanical properties at different scale length was attributed to the porosity, CNT clustering, CNT-splat adhesion and Al4C3 formation at the CNT/matrix interface. The Dispersion parameter (DP) was more sensitive than Clustering parameter (CP) in measuring degree of CNT distribution in the matrix.

Development of functionalised multiwalled carbon nanotube/polyaniline composites for electrical applications

Combining intrinsically conducting polymers with carbon nanotubes (CNT) helps in creating composites with superior electrical and thermal characteristics. These composites are capable of replacing metals and semiconductors as they possess unique combination of electrical conductivity, flexibility, stretchability, softness and bio-compatibility. Their potential for use in various organic devices such as super capacitors, printable conductors, optoelectronic devices, sensors, actuators, electrochemical devices, electromagnetic interference shielding, field effect transistors, LEDs, thermoelectrics etc. makes them excellent substitutes for present day semiconductors.However, many of these potential applications have not been fully exploited because of various open–ended challenges. Composites meant for use in organic devices require highly stable conductivity for the longevity of the devices. CNT when incorporated at specific proportions, and with special methods contributes quite positively to this end.The increasing demand for energy and depleting fossil fuel reserves has broadened the scope for research into alternative energy sources. A unique and efficient method for harnessing energy is thermoelectric energy conversion method. Here, heat is converted directly into electricity using a class of materials known as thermoelectric materials. Though polymers have low electrical conductivity and thermo power, their low thermal conductivity favours use as a thermoelectric material. The thermally disconnected, but electrically connected carrier pathways in CNT/Polymer composites can satisfy the so-called “phonon-glass/electron-crystal” property required for thermoelectric materials. Strain sensing is commonly used for monitoring in engineering, medicine, space or ocean research. Polymeric composites are ideal candidates for the manufacture of strain sensors. Conducting elastomeric composites containing CNT are widely used for this application. These CNT/Polymer composites offer resistance change over a large strain range due to the low Young‟s modulus and higher elasticity. They are also capable of covering surfaces with arbitrary curvatures.Due to the high operating frequency and bandwidth of electronic equipments electromagnetic interference (EMI) has attained the tag of an „environmental pollutant‟, affecting other electronic devices as well as living organisms. Among the EMI shielding materials, polymer composites based on carbon nanotubes show great promise. High strength and stiffness, extremely high aspect ratio, and good electrical conductivity of CNT make it a filler of choice for shielding applications. A method for better dispersion, orientation and connectivity of the CNT in polymer matrix is required to enhance conductivity and EMI shielding. This thesis presents a detailed study on the synthesis of functionalised multiwalled carbon nanotube/polyaniline composites and their application in electronic devices. The major areas focused include DC conductivity retention at high temperature, thermoelectric, strain sensing and electromagnetic interference shielding properties, thermogravimetric, dynamic mechanical and tensile analysis in addition to structural and morphological studies.

CHARACTERIZATION OF THERMAL AND MECHANICAL PROPERTIES OF POLYPROPYLENE–BASED COMPOSITES FOR FUEL CELL BIPOLAR PLATES AND DEVELOPMENT OF EDUCATIONAL TOOLS IN HYDROGEN AND FUEL CELL TECHNOLOGIES

In this project we developed conductive thermoplastic resins by adding varying amounts of three different carbon fillers: carbon black (CB), synthetic graphite (SG) and multi–walled carbon nanotubes (CNT) to a polypropylene matrix for application as fuel cell bipolar plates. This component of fuel cells provides mechanical support to the stack, circulates the gases that participate in the electrochemical reaction within the fuel cell and allows for removal of the excess heat from the system. The materials fabricated in this work were tested to determine their mechanical and thermal properties. These materials were produced by adding varying amounts of single carbon fillers to a polypropylene matrix (2.5 to 15 wt.% Ketjenblack EC-600 JD carbon black, 10 to 80 wt.% Asbury Carbons’ Thermocarb TC-300 synthetic graphite, and 2.5 to 15 wt.% of Hyperion Catalysis International’s FIBRILTM multi-walled carbon nanotubes) In addition, composite materials containing combinations of these three fillers were produced. The thermal conductivity results showed an increase in both through–plane and in–plane thermal conductivities, with the largest increase observed for synthetic graphite. The Department of Energy (DOE) had previously set a thermal conductivity goal of 20 W/m·K, which was surpassed by formulations containing 75 wt.% and 80 wt.% SG, yielding in–plane thermal conductivity values of 24.4 W/m·K and 33.6 W/m·K, respectively. In addition, composites containing 2.5 wt.% CB, 65 wt.% SG, and 6 wt.% CNT in PP had an in–plane thermal conductivity of 37 W/m·K. Flexural and tensile tests were conducted. All composite formulations exceeded the flexural strength target of 25 MPa set by DOE. The tensile and flexural modulus of the composites increased with higher concentration of carbon fillers. Carbon black and synthetic graphite caused a decrease in the tensile and flexural strengths of the composites. However, carbon nanotubes increased the composite tensile and flexural strengths. Mathematical models were applied to estimate through–plane and in–plane thermal conductivities of single and multiple filler formulations, and tensile modulus of single–filler formulations. For thermal conductivity, Nielsen’s model yielded accurate thermal conductivity values when compared to experimental results obtained through the Flash method. For prediction of tensile modulus Nielsen’s model yielded the smallest error between the predicted and experimental values. The second part of this project consisted of the development of a curriculum in Fuel Cell and Hydrogen Technologies to address different educational barriers identified by the Department of Energy. By the creation of new courses and enterprise programs in the areas of fuel cells and the use of hydrogen as an energy carrier, we introduced engineering students to the new technologies, policies and challenges present with this alternative energy. Feedback provided by students participating in these courses and enterprise programs indicate positive acceptance of the different educational tools. Results obtained from a survey applied to students after participating in these courses showed an increase in the knowledge and awareness of energy fundamentals, which indicates the modules developed in this project are effective in introducing students to alternative energy sources.

Effect Of 4-(n,n-dimethylamino)phenethyl Alcohol On Degree Of Conversion And Cytotoxicity Of Photo-polymerized Cq-based Resin Composites.

The aim of this study was to evaluate the degree of conversion (DC) and the cytotoxicity of photo-cured experimental resin composites containing 4-(N,N-dimethylamino)phenethyl alcohol (DMPOH) combined to the camphorquinone (CQ) compared with ethylamine benzoate (EDAB). The resin composites were mechanically blended using 35 wt% of an organic matrix and 65 wt% of filler loading. To this matrix was added 0.2 wt% of CQ and 0.2 wt% of one of the reducing agents tested. 5x1 mm samples (n=5) were previously submitted to DC measurement and then pre-immersed in complete culture medium without 10% (v/v) bovine serum for 1 h or 24 h at 37 °C in a humidifier incubator with 5% CO2 and 95% humidity to evaluate the cytotoxic effects of experimental resin composites using the MTT assay on immortalized human keratinocytes cells. As a result of absence of normal distribution, the statistical analysis was performed using the nonparametric Kruskal-Wallis to evaluate the cytotoxicity and one-way analysis of variance to evaluate the DC. For multiple comparisons, cytotoxicity statistical analyses were submitted to Student-Newman-Keuls and DC analysis to Tukey's HSD post-hoc test (=0.05). No significant differences were found between the DC of DMPOH (49.9%) and EDAB (50.7%). 1 h outcomes showed no significant difference of the cell viability between EDAB (99.26%), DMPOH (94.85%) and the control group (100%). After 24 h no significant difference were found between EDAB (48.44%) and DMPOH (38.06%), but significant difference was found compared with the control group (p>0.05). DMPOH presented similar DC and cytotoxicity compared with EDAB when associated with CQ.

Polymerization shrinkage stress of composites photoactivated by different light sources

The purpose of this study was to compare the polymerization shrinkage stress of composite resins (microfilled, microhybrid and hybrid) photoactivated by quartz-tungsten halogen light (QTH) and light-emitting diode (LED). Glass rods (5.0 mm x 5.0 cm) were fabricated and had one of the surfaces air-abraded with aluminum oxide and coated with a layer of an adhesive system, which was photoactivated with the QTH unit. The glass rods were vertically assembled, in pairs, to a universal testing machine and the composites were applied to the lower rod. The upper rod was placed closer, at 2 mm, and an extensometer was attached to the rods. The 20 composites were polymerized by either QTH (n=10) or LED (n=10) curing units. Polymerization was carried out using 2 devices positioned in opposite sides, which were simultaneously activated for 40 s. Shrinkage stress was analyzed twice: shortly after polymerization (t40s) and 10 min later (t10min). Data were analyzed statistically by 2-way ANOVA and Tukey's test (a=5%). The shrinkage stress for all composites was higher at t10min than at t40s, regardless of the activation source. Microfilled composite resins showed lower shrinkage stress values compared to the other composite resins. For the hybrid and microhybrid composite resins, the light source had no influence on the shrinkage stress, except for microfilled composite at t10min. It may be concluded that the composition of composite resins is the factor with the strongest influence on shrinkage stress.

Effect of staining solutions and repolishing on color stability of direct composites

OBJECTIVES: The purpose of this study was to assess the color change of three types of composite resins exposed to coffee and cola drink, and the effect of repolishing on the color stability of these composites after staining. MATERIALS AND METHODS: Fifteen specimens (15 mm diameter and 2 mm thick) were fabricated from microhybrid (Esthet-X; Dentsply and Filtek Z-250; 3M ESPE) and high-density hybrid (Surefil; Dentsply) composites, and were finished and polished with aluminum oxide discs (Sof-Lex; 3M ESPE). Color of the specimens was measured according to the CIE L*a*b* system in a refection spectrophotometer (PCB 6807; BYK Gardner). After baseline color measurements, 5 specimens of each resin were immersed in different staining solutions for 15 days: G1 - distilled water (control), G2 - coffee, G3 - cola soft drink. Afterwards, new color measurement was performed and the specimens were repolished and submitted to new color reading. Color stability was determined by the difference (ΔE) between the coordinates L*, a*, and b* obtained from the specimens before and after immersion into the solutions and after repolishing. RESULTS: There was no statistically signifcant difference (ANOVA, Tukey's test; p>0.05) among the ΔE values for the different types of composites after staining or repolishing. For all composite resins, coffee promoted more color change (ΔE>3.3) than distilled water and the cola soft drink. After repolishing, the ΔE values of the specimens immersed in coffee decreased to clinically acceptable values (ΔE<3.3), but remained signifcantly higher than those of the other groups. CONCLUSIONS: No signifcant difference was found among composite resins or between color values before and after repolishing of specimens immersed in distilled water and cola. Immersing specimens in coffee caused greater color change in all types of composite resins tested in this study and repolishing contributed to decrease staining to clinically acceptable ΔE values.

Microhardness assessment of different commercial brands of resin composites with different degrees of translucence

Owing to improvements in its mechanical properties and to the availability of shade and translucence resources, resin composite has become one of the most widely used restorative materials in present day Dentistry. The aim of this study was to assess the relation between the surface hardness of seven different commercial brands of resin composites (Charisma, Fill Magic, Master Fill, Natural Look, Opallis, Tetric Ceram, and Z250) and the different degrees of translucence (translucid, enamel and dentin). Vickers microhardness testing revealed significant differences among the groups. Z250 was the commercial brand that showed the best performance in the hardness test. When comparing the three groups assessed within the same brand, only Master Fill and Fill Magic presented statistically significant differences among all of the different translucencies. Natural Look was the only one that showed no significant difference among any of the three groups. Charisma, Opallis, Tetric Ceram and Z250 showed significant differences among some of the tested groups. Based on the results found in this study, it was not possible to establish a relation between translucence and the microhardness of the resin composites assessed. Depending on the material assessed, however, translucence variation did affect the microhardness values of the resin composites.

Effect of different polishing systems on the surface roughness of microhybrid composites

The use of composite resins in dentistry is well accepted for restoring anterior and posterior teeth. Many polishing protocols have been evaluated for their effect on the surface roughness of restorative materials. This study compared the effect of different polishing systems on the surface roughness of microhybrid composites. Thirty-six specimens were prepared for each composite $#91;Charisma® (Heraeus Kulzer), Fill Magic® (Vigodent), TPH Spectrum® (Dentsply), Z100® (3M/ESPE) and Z250® (3M/ESPE)] and submitted to surface treatment with Enhance® and PoGo® (Dentsply) points, sequential Sof-Lex XT® aluminum oxide disks (3M/ESPE), and felt disks (TDV) combined with Excel® diamond polishing paste (TDV). Average surface roughness (Ra) was measured with a mechanical roughness tester. The data were analyzed by two-way ANOVA with repetition of the factorial design and the Tukey-Kramer test (p<0.01). The F-test result for treatments and resins was high (p<0.0001 for both), indicating that the effect of the treatment applied to the specimen surface and the effect of the type of resin on surface roughness was highly significant. Regarding the interaction between polishing system and type of resin used, a p value of 0.0002 was obtained, indicating a statistically significant difference. A Ra of 1.3663 was obtained for the Sof-Lex/TPH Spectrum interaction. In contrast, the Ra for the felt disk+paste/Z250 interactions was 0.1846. In conclusion, Sof-Lex polishing system produced a higher surface roughness on TPH Spectrum resin when compared to the other interactions.

Flexural strength and hardness of direct and indirect composites

The objective of this study was to evaluate the flexural strength (σf) and hardness (H) of direct and indirect composites, testing the hypotheses that direct resin composites produce higher σf and H values than indirect composites and that these properties are positively related. Ten bar-shaped specimens (25 mm x 2 mm x 2 mm) were fabricated for each direct [D250 - Filtek Z250 (3M-Espe) and D350 - Filtek Z350 (3M-Espe)] and indirect [ISin - Sinfony (3M-Espe) and IVM - VitaVM LC (Vita Zahnfabrik)] materials, according to the manufacturer's instructions and ISO4049 specifications. The σf was tested in three-point bending using a universal testing machine (EMIC DL 2000) at a crosshead speed of 0.5 mm/min (ISO4049). Knoop hardness (H) was measured on the specimens' fragments resultant from the σf test and calculated as H = 14.2P/l², where P is the applied load (0.1 kg; dwell time = 15 s) and l is the longest diagonal of the diamond shaped indent (ASTM E384). The data were statistically analyzed using Anova and Tukey tests (α = 0.05). The mean σf and standard deviation values (MPa) and statistical grouping were: D250 - 135.4 ± 17.6a; D350 - 123.7 ± 11.1b; ISin - 98.4 ± 6.4c; IVM - 73.1 ± 4.9d. The mean H and standard deviation values (kg/mm²) and statistical grouping were: D250 - 98.12 ± 1.8a; D350 - 86.5 ± 1.9b; ISin - 28.3 ± 0.9c; IVM - 30.8 ± 1.0c. The direct composite systems examined produce higher mean σf and H values than the indirect composites, and the mean values of these properties were positively correlated (r = 0.91), confirming the study hypotheses.