Evaluation of degree of conversion and hardness of dental composites photo-activated with different light guide tips

Objective: The aim of this study was to evaluate the degree of conversion and hardness of different composite resins, photo-activated for 40 s with two different light guide tips, fiber optic and polymer. Methods: Five specimens were made for each group evaluated. The percentage of unreacted carbon double bonds (% C=C) was determined from the ratio of absorbance intensities of aliphatic C=C (peak at 1637 cm-1) against internal standard before and after curing of the specimen: aromatic C-C (peak at 1610 cm-1). The Vickers hardness measurements were performed in a universal testing machine. A 50 gf load was used and the indenter with a dwell time of 30 seconds. The degree of conversion and hardness mean values were analyzed separately by ANOVA and Tukey's test, with a significance level set at 5%. Results: The mean values of degree of conversion for the polymer and fiber optic light guide tip were statistically different (P<.001). The hardness mean values were statistically different among the light guide tips (P<.001), but also there was difference between top and bottom surfaces (P<.001). Conclusions: The results showed that the resins photo-activated with the fiber optic light guide tip promoted higher values for degree of conversion and hardness.

Preparation and characterisation of refractory whiskers and selected alumina composites

A whisker is a common name of single crystalline inorganic fibre of small dimensions, typically 0.5-1 μm in diameter and 20-50 μm in length. Whiskers are mainly used as reinforcement of ceramics. This work describes the synthesis and characterisation of new whisker types. Ti0.33Ta0.33Nb0.33CxN1-x, TiB2, B4C, and LaxCe1-xB6 have been prepared by carbothermal vapour–liquid–solid (CTR-VLS) growth mechanisms in the temperature range 900-1800°C, in argon or nitrogen. Generally, carbon and different suitable oxides were used as whisker precursors. The oxides reacted via a carbothermal reduction process. A halogenide salt was added to form gaseous metal halogenides or oxohalogenides and small amount of a transition metal was added to catalyse the whisker growth. In this mechanism, the whisker constituents are dissolved into the catalyst, in liquid phase, which becomes supersaturated. Then a whisker could nucleate and grow out under continuous feed of constituents. The syntheses of TiC, TiB2, and B4C were followed at ordinary synthesis conditions by means of mass spectrometry (MS), thermogravimetry (TG), differential thermal analysis (DTA) and quenching. The main reaction starting temperatures and reaction time for the different mixtures was revealed, and it was found that the temperature inside the crucible during the reactions was up to 100°C below the furnace set-point, due to endothermic nature of the reactions. Quench experiments showed that whiskers were formed already when reaching the temperature plateau, but the yield increased fast with the holding time and reached a maximum after about 20-30 minutes. Growth models for whisker formation have been proposed. Alumina based composites reinforced by (2-5 vol.%) TiCnano and TiNnano and 25 vol.% of carbide, and boride phases (whiskers and particulates of TiC, TiN, TaC, NbC, (Ti,Ta)C, (Ti,Ta,Nb)C, SiC, TiB2 and B4C) have been prepared by a developed aqueous colloidal processing route followed by hot pressing for 90 min at 1700°C, 28 MPa or SPS sintering for 5 minutes at 1200-1600°C and 75 MPa. Vickers indentation measurements showed that the lowest possible sintering temperature is to prefer from mechanical properties point of view. In the TiNnano composites the fracture mode was typically intergranular, while it was transgranular in the SiCnano composites. The whisker and particulate composites have been compared in terms of e.g. microstructure and mechanical properties. Generally, additions of whiskers yielded higher fracture toughness compared to particulates. Composites of commercially available SiC whiskers showed best mechanical properties with a low spread but all the other whisker phases, especially TiB2, exhibited a great potential as reinforcement materials.

Active fibre-reinforced composites with embedded shape memory alloys

This dissertation concerns active fibre-reinforced composites with embedded shape memory alloy wires. The structural application of active materials allows to develop adaptive structures which actively respond to changes in the environment, such as morphing structures, self-healing structures and power harvesting devices. In particular, shape memory alloy actuators integrated within a composite actively control the structural shape or stiffness, thus influencing the composite static and dynamic properties. Envisaged applications include, among others, the prevention of thermal buckling of the outer skin of air vehicles, shape changes in panels for improved aerodynamic characteristics and the deployment of large space structures. The study and design of active composites is a complex and multidisciplinary topic, requiring in-depth understanding of both the coupled behaviour of active materials and the interaction between the different composite constituents. Both fibre-reinforced composites and shape memory alloys are extremely active research topics, whose modelling and experimental characterisation still present a number of open problems. Thus, while this dissertation focuses on active composites, some of the research results presented here can be usefully applied to traditional fibre-reinforced composites or other shape memory alloy applications. The dissertation is composed of four chapters. In the first chapter, active fibre-reinforced composites are introduced by giving an overview of the most common choices available for the reinforcement, matrix and production process, together with a brief introduction and classification of active materials. The second chapter presents a number of original contributions regarding the modelling of fibre-reinforced composites. Different two-dimensional laminate theories are derived from a parent three-dimensional theory, introducing a procedure for the a posteriori reconstruction of transverse stresses along the laminate thickness. Accurate through the thickness stresses are crucial for the composite modelling as they are responsible for some common failure mechanisms. A new finite element based on the First-order Shear Deformation Theory and a hybrid stress approach is proposed for the numerical solution of the two-dimensional laminate problem. The element is simple and computationally efficient. The transverse stresses through the laminate thickness are reconstructed starting from a general finite element solution. A two stages procedure is devised, based on Recovery by Compatibility in Patches and three-dimensional equilibrium. Finally, the determination of the elastic parameters of laminated structures via numerical-experimental Bayesian techniques is investigated. Two different estimators are analysed and compared, leading to the definition of an alternative procedure to improve convergence of the estimation process. The third chapter focuses on shape memory alloys, describing their properties and applications. A number of constitutive models proposed in the literature, both one-dimensional and three-dimensional, are critically discussed and compared, underlining their potential and limitations, which are mainly related to the definition of the phase diagram and the choice of internal variables. Some new experimental results on shape memory alloy material characterisation are also presented. These experimental observations display some features of the shape memory alloy behaviour which are generally not included in the current models, thus some ideas are proposed for the development of a new constitutive model. The fourth chapter, finally, focuses on active composite plates with embedded shape memory alloy wires. A number of di®erent approaches can be used to predict the behaviour of such structures, each model presenting different advantages and drawbacks related to complexity and versatility. A simple model able to describe both shape and stiffness control configurations within the same context is proposed and implemented. The model is then validated considering the shape control configuration, which is the most sensitive to model parameters. The experimental work is divided in two parts. In the first part, an active composite is built by gluing prestrained shape memory alloy wires on a carbon fibre laminate strip. This structure is relatively simple to build, however it is useful in order to experimentally demonstrate the feasibility of the concept proposed in the first part of the chapter. In the second part, the making of a fibre-reinforced composite with embedded shape memory alloy wires is investigated, considering different possible choices of materials and manufacturing processes. Although a number of technological issues still need to be faced, the experimental results allow to demonstrate the mechanism of shape control via embedded shape memory alloy wires, while showing a good agreement with the proposed model predictions.

Conductive Polymer Composites

In recent years, nanotechnologies have led to the production of materials with new and sometimes unexpected qualities through the manipulation of nanoscale components. This research aimed primarily to the study of the correlation between hierarchical structures of hybrid organic-inorganic materials such as conductive polymer composites (CPCs). Using a bottom-up methodology, we could synthesize a wide range of inorganic nanometric materials with a high degree of homogeneity and purity, such as thiol capped metal nanoparticles, stoichiometric geomimetic chrysotile nanotubes and metal dioxide nanoparticles. It was also possible to produce inorganic systems formed from the interaction between the synthesized materials. These synthesized materials and others like multiwalled carbon nanotubes and grapheme oxide were used to produce conductive polymer composites. Electrospinning causes polymer fibers to become elongated using an electric field. This technique was used to produce fibers with a nanometric diameter of a polymer blend based on two different intrinsically conducting polymers polymers (ICPs): polyaniline (PANI) and poly(3-hexylthiophene) (P3HT). Using different materials as second phase in the initial electrospun polymer fibers caused significant changes to the material hierarchical structure, leading to the creation of CPCs with modified electrical properties. Further study of the properties of these new materials resulted in a better understanding of the electrical conductivity mechanisms in these electrospun materials.

In-plane thermal conductivity modeling of carbon filled liquid crystal polymer based resins

Adding conductive carbon fillers to insulating thermoplastic resins increases composite electrical and thermal conductivity. Often, as much of a single type of carbon filler is added to achieve the desired conductivity, while still allowing the material to be molded into a bipolar plate for a fuel cell. In this study, varying amounts of three different carbons (carbon black, synthetic graphite particles, and carbon fiber) were added to Vectra A950RX Liquid Crystal Polymer. The in-plane thermal conductivity of the resulting single filler composites were tested. The results showed that adding synthetic graphite particles caused the largest increase in the in-plane thermal conductivity of the composite. The composites were modeled using ellipsoidal inclusion problems to predict the effective in-plane thermal conductivities at varying volume fractions with only physical property data of constituents. The synthetic graphite and carbon black were modeled using the average field approximation with ellipsoidal inclusions and the model showed good agreement with the experimental data. The carbon fiber polymer composite was modeled using an assemblage of coated ellipsoids and the model showed good agreement with the experimental data.

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.

Tuning the properties of carbon fiber-reinforced poly (phenylene sulphide) laminates via incorporation of inorganic fullerene-like WS2 nanoparticles

Novel carbon fiber (CF)-reinforced poly(phenylene sulphide) (PPS) laminates incorporating inorganic fullerene-like tungsten disulfide (IF-WS2) nanoparticles were prepared via melt-blending and hot-press processing. The influence of the IF-WS2 on the morphology, thermal, mechanical and tribological properties of PPS/CF composites was investigated. Efficient nanoparticle dispersion within the matrix was attained without using surfactants. A progressive rise in thermal stability was found with increasing IF-WS2 loading, as revealed by thermogravimetric analysis. The addition of low nanoparticle contents retarded the crystallization of the matrix, whereas concentrations equal or higher than 1.0 wt% increased both the crystallization temperature and degree of crystallinity compared to those of PPS/CF. Mechanical tests indicated that with only 1.0 wt% IF-WS2 the flexural modulus and strength of PPS/CF improved by 17 and 14%, respectively, without loss in toughness, ascribed to a synergistic effect between the two fillers. A significant enhancement in the storage modulus and glass transition temperature was also observed. Moreover, the wear rate and coefficient of friction strongly decreased, attributed to the lubricant role of the IF-WS2 combined with their reinforcing effect. These inorganic nanoparticles show great potential to improve the mechanical and tribological properties of conventional thermoplastic/CF composites for structural applications.

Inorganic Nanoparticle-Modified Poly(Phenylene Sulphide)/ Carbon Fiber Laminates: Thermomechanical Behaviour

Carbon fiber (CF)-reinforced high-temperature thermoplastics such as poly(phenylene sulphide) (PPS) are widely used in structural composites for aerospace and automotive applications. The porosity of CF-reinforced polymers is a very important topic for practical applications since there is a direct correlation between void content and mechanical properties. In this study, inorganic fullerene-like tungsten disulphide (IF-WS2) lubricant nanoparticles were used to manufacture PPS/IF-WS2/CF laminates via melt-blending and hot-press processing, and the effect of IF-WS2 loading on the quality, thermal and mechanical behaviour of the hybrid composites was investigated. The addition of IF-WS2 improved fiber impregnation, resulting in lower degree of porosity and increased delamination resistance, compression and flexural properties; their reinforcement effect was greater at temperatures above the glass transition (Tg). IF-WS2 contents higher than 0.5 wt % increased Tg and the heat deflection temperature while reduced the coefficient of thermal expansion. The multiscale laminates exhibited higher ignition point and notably reduced peak heat release rate compared to PPS/CF. The coexistence of micro- and nano-scale fillers resulted in synergistic effects that enhanced the stiffness, strength, thermal conductivity and flame retardancy of the matrix. The results presented herein demonstrate that the IF-WS2 are very promising nanofillers to improve the thermomechanical properties of conventional thermoplastic/CF composites.

Optimization of curing cycle in carbon fiber-reinforced laminates: Void distribution and mechanical properties

A strategy is presented to optimize out-of-autoclave processing of quasi-isotropic carbon fiber-reinforced laminates. Square panels of 4.6 mm nominal thickness with very low porosity ð6 0:2%Þ were manufactured by compression molding at low pressure (0.2 MPa) by careful design of the temperature cycle to maximize the processing window. The mechanisms of void migration during processing were ascertained by means of X-ray microtomography and the effect of ply clustering on porosity and on void shape was explained. Finally, the effect of porosity and ply clustering on the compressive strength before and after impact was studied.

X-ray microtomography analysis of the damage micromechanisms in 3D woven composites under low-velocity impact

3D woven composites reinforced with either S2 glass, carbon or a hybrid combination of both and containing either polyethylene or carbon z-yarns were tested under low-velocity impact. Different impact energies (in the range of 21–316 J) were used and the mechanical response (in terms of the impact strength and energy dissipated) was compared with that measured in high-performance, albeit standard, 2D laminates. It was found that the impact strength in both 2D and 3D materials was mainly dependent on the in-plane fiber fracture. Conversely, the energy absorption capability was primarily influenced by the presence of z-yarns, having the 3D composites dissipated over twice the energy than the 2D laminates, irrespective of their individual characteristics (fiber type, compaction degree, porosity, etc.). X-ray microtomography revealed that this improvement was due to the z-yarns, which delayed delamination and maintained the structural integrity of the laminate, promoting energy dissipation by tow splitting, intensive fiber breakage under the tup and formation of a plug by out-of-plane shear.

Bending reinforcement of timber beams with composite carbon fiber and basalt fiber materials

En el presente trabajo se lleva a cabo un estudio basado en datos obtenidos experimentalmente mediante el ensayo a flexión de vigas de madera de pino silvestre reforzadas con materiales compuestos. Las fibras que componen los tejidos utilizados para la ejecución de los refuerzos son de basalto y de carbono. En el caso de los compuestos de fibra de basalto se aplican en distintos gramajes, y los de carbono en tejido unidireccional y bidireccional. El material compuesto se realizó in situ, simultáneamente a la ejecución del refuerzo. Se aplicaron en una y en dos capas, según el caso, y la forma de colocación fue en ?U?, adhiriéndose al canto inferior y a las caras laterales de la viga mediante resina o mortero epoxi. Se analiza el comportamiento de las vigas según las variables de refuerzo aplicadas y se comparan con los resultados de vigas ensayadas sin reforzar. Con este trabajo queda demostrado el buen funcionamiento del FRP de fibra de basalto aplicado en el refuerzo de vigas de madera y de los tejidos de carbono bidireccionales con respecto a los unidireccionales.

Mechanical behavior and failure micromechanisms of hybrid 3D woven composites in tension

The deformation and failure micromechanisms of a hybrid 3D woven composite were studied in tension. Plain and open-hole composite coupons were tested in tension until failure in the fill and warp directions, as well as fiber tows extracted from the dry fabric and impregnated with the matrix. The macroscopic evolution of damage in the composite coupons was assessed by means of periodic unloading–reloading (to obtain the elastic modulus and the residual strain), whereas the microscopic mechanism were established by means of X-ray computed microtomography. To this end, specimens were periodically removed from the mechanical testing machine and infiltrated with ZnI-containing liquid to assess the main damage modes as a function of the applied strain. The experimental observations and the predictions of an isostrain model were used to understand the key factors controlling the elastic modulus, strength and notch sensitivity of hybrid 3D woven composites in tension. It was found that the full contribution of the glass fibers to the composite strength was not employed, due to the premature fracture of the carbon fibers, but their presence increased the fracture strain and the energy dissipated during fracture. Thus, hybridization of the 3D woven composite led to a notch-insensitive behavior as demonstrated by open-hole tests

Automatic quantification of matrix cracking and fiber rotation by X-ray computed tomography in shear-deformed carbon fiber-reinforced laminates

The deformation and damage mechanisms of carbon fiber-reinforced epoxy laminates deformed in shear were studied by means of X-ray computed tomography. In particular, the evolution of matrix cracking, interply delamination and fiber rotation was ascertained as a function of the applied strain. In order to provide quantitative information, an algorithm was developed to automatically determine the crack density and the fiber orientation from the tomograms. The investigation provided new insights about the complex interaction between the different damage mechanisms (i.e. matrix cracking and interply delamination) as a function of the applied strain, ply thickness and ply location within the laminate as well as quantitative data about the evolution of matrix cracking and fiber rotation during deformation

Hierarchical and hybrid polymer nanocomposites based on carbon nanotubes and inorganic fullerene type nanoparticles

The influence of singlewalled carbon nanotubes (SWCNT) and inorganic fullerenelike tungsten disulfide nanoparticles (IFWS2) on the morphology and thermal, mechanical and electrical performance of multifunctional fibrereinforced polymer composites has been investigated. Significant improvements were observed in stiffness, strength and toughness in poly (ether ether ketone) (PEEK) / (SWCNT) / glass fibre (GF) laminates when a compatibilizer was used for wrapping the CNTs. Hybrid poly(phenylene sulphide) (PPS)/IFWS2/ carbon fibre (CF) reinforced polymer composites showed improved mechanical and tribological properties attributed to a synergetic effect between the IF nanoparticles and CF.

Multifunctional cement composites strain and damage sensors applied on reinforced concrete (RC) structural elements

In this research, strain-sensing and damage-sensing functional properties of cement composites have been studied on a conventional reinforced concrete (RC) beam. Carbon nanofiber (CNFCC) and fiber (CFCC) cement composites were used as sensors on a 4 m long RC beam. Different casting conditions (in situ or attached), service location (under tension or compression) and electrical contacts (embedded or superficial) were compared. Both CNFCC and CFCC were suitable as strain sensors in reversible (elastic) sensing condition testing. CNFCC showed higher sensitivities (gage factor up to 191.8), while CFCC only reached gage factors values of 178.9 (tension) or 49.5 (compression). Furthermore, damage-sensing tests were run, increasing the applied load progressively up to the RC beam failure. In these conditions, CNFCC sensors were also strain sensitive, but no damage sensing mechanism was detected for the strain levels achieved during the tests. Hence, these cement composites could act as strain sensors, even for severe damaged structures near to their collapse.