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In the last years, bistable composite structures are finding interest in several aeronautical applications such as power harvesting devices or morphing applications on very small aircraft/drones, not needing servo-activated control systems. Residual stresses, developed upon cooling after curing, leads to warped the composite laminates. Several batches of unsymmetrical and unbalanced [0°/90°] laminates were cured in an autoclave according to a standard temperature cycle, following the pre-preg supplier suggested curing cycle. In order to increase the thermal stresses (and hence the bistability phenomenon), these laminates were removed from the autoclave immediately after the curing reaction and rapidly cooled down at room temperature not applying the indicated cool rate between 2 and 5 °C min−1. During storage at room temperature, thermal stresses changed over time, indicating that asymptotic stress relaxation occurs. The first part of this work looks at residual stress characterization of bistable composite plates measuring the changes of shape observed during room temperature annealing. Rectangular plates were produced and the bistable geometric shapes were accurately assessed using a laser scanner system over several days, in order to monitor the curvature changes due to stress relaxation. Then phenomenological viscoelastic predicting models were proposed for a quick estimate for the strain/stress relaxation phenomenon. The loss of bistability was demonstrated with the help of numerical simulation and experimental testing. The final goal was to gain a better knowledge of the relation between processing and final shape of bistable laminates, in order to make them suitable for application on small air vehicles.

This work contributes to fill one of the gaps regarding nanoplastic interactions with biological systems by producing polyethylene terephthalate (PET) model nanoplastics, similar to those found in the marine environment, by means of a fast top-down approach based on mechanical fragmentation. Their size distribution and morphology were characterized by laser diffraction and atomic force microscopy (AFM). Their autofluorescence was studied by spectrofluorimetry and fluorescence imaging, being a key property for the evaluation of their interaction with biota. The emission spectra of label-free nanoplastics were comparable with those of PET nanoplastics labeled with Nile red. Finally, the suitability of label-free nanoplastics for biological studies was assessed by in vitro exposure with Mytilus galloprovincialis hemolymphatic cells in a time interval up to 6 h. The nanoplastic internalization into these cells, known to be provided with phagocytic activity, was assessed by fluorescence microscopy. The obtained results underlined that the autofluorescence of the model PET nanoplastics produced in the laboratory was adequate for biological studies having the potential to overcome the disadvantages commonly associated with several fluorescent dyes, such as the tendency to also stain other organic materials different from plastics, to form aggregates due to intermolecular interactions at high concentrations with a consequent decrease in fluorescence intensity, and to dye desorption from nanoparticles. The results of the autofluorescence study provide an innovative approach for plastic risk assessment.

In this work, a potentially economic and environmentally friendly method for the synthesis of bacterial cellulose (BC) by Gluconacetobacter xylinus from a biomass containing orange peel extract was evaluated. Orange peel extract was used as a culture medium without any hydrolysis treatment, thus speeding up the synthesis procedure. The efficacy of orange peel as a carbon source was compared with that of sucrose. The orange peel extract formed thicker cellulose gels than those formed using sucrose. X-ray diffraction (XRD) revealed both a high crystallinity index and crystallite size of BC nanofibers in samples obtained from orange peel (BC_Orange). Field emission scanning electron microscopy (FE-SEM) revealed a highly densely packed nanofibrous structure (50 nm in diameter). BC_Orange presented a two-fold increase in water holding capacity (WHC), and dynamic mechanical analysis (DMA) showed a 44% increase in storage modulus compared to sucrose derived BC. These results showed that the naturally available carbon sources derived from orange peel extract can be effectively used for BC production. The orange-based culture medium can be considered a profitable alternative to the generation of high-value products in a virtuous circular economy model.

Heritage buildings worldwide are primarily masonry construction. Over the centuries, these structures have demonstrated a high vulnerability in seismic events. The seismic protection and retrofitting of these historical structures require an effective structural solution, without compromise, cover or loss of architectural and artistic value. For these scenarios, the use of Fiber Reinforced Polymers (FRPs) is discouraged since removability of the intervention is often a mandatory requirement, and the polymeric adhesives bond the fiber to the masonry substrate, eliminating the possibility of preserving the underlying material during a replacement operation. In FRP-strengthening, the force transfer from the substrate to the FRP occurs by means of bond stresses. However, in the case of column confinement, while full bond is nevertheless developed through the adhesive, it is not necessary for the effectiveness of the confinement. Instead, the confining pressure is applied by the FRP when transversal dilatation of the column is mobilized. Thus, with the exception of the overlapping regions, an FRP retrofit for column confinement works due to a contact phenomenon instead of bond. In this context, new FRP-confinement techniques, based on contact rather than adhesion, can be developed. This paper presents research on fully-reversible contact-based techniques for FRP-confinement. Three different techniques were developed and demonstrated by the authors. Each technique was experimentally evaluated through compression tests of small-scale limestone cylinders. The reversibility of each technique was verified through comparison of the substrates before the FRP-confinement and after the testing. The effectiveness of each technique was evaluated by comparing the compressive strength and the deformability with those obtained for unconfined specimens. The concepts show promise as effective and reversible strengthening techniques.

The high PET production volume and the waste mismanagement of PET litter make it one of the most polluting plastic material. Its diffusion in marine litter is widely assessed according to public opinion and documented in the literature. The major sources of PET microplastics in the marine environment are bottles and fibers. The role of PET micro/nanoplastics of vector of toxic chemicals, their fate and the negative effects on the environment and human health is still under discussion.

Carbon fiber-epoxy thin laminates, manufactured adopting a [0/90] non-symmetric lay-up, are characterized by two stable curved shapes, so being bistable. These composite thin laminates are attracting great interest for their potential application as novel morphing structures and power harvesting devices in many engineering fields. The curvature changes of rectangular bistable plates were monitored at room temperature by a laser scanner system over a time span of 10 d. These changes were ascribed to the relaxation of thermal stresses over time. Anisotropic stress relaxation behavior was then studied looking at the matrix dominated properties, such as the transverse modulus in accelerated high temperature experiments and the moisture absorption. Then, a simple viscoelastic model was proposed together with a finite element analysis of the distortion arising from laminate cooling at the end of high temperature cure process. The experimental and numerical results showed that the transverse elastic modulus and the hygroscopic effect are the main factors affecting the shape relaxation of bistable laminates.

Liquid resin infusion processes are becoming attractive for aeronautic applications as an alternative to conventional autoclave-based processes. They still present several challenges, which can be faced only with an accurate simulation able to optimize the process parameters and to replace traditional time-consuming trial-and-error procedures. This paper presents an experimentally validated model to simulate the resin infusion process of an aeronautical component by accounting for the anisotropic permeability of the reinforcement and the chemophysical and rheological changes in the crosslinking resin. The input parameters of the model have been experimentally determined. The experimental work has been devoted to the study of the curing kinetics and chemorheological behavior of the thermosetting epoxy matrix and to the determination of both the in-plane and out-of-plane permeability of two carbon fiber preforms using an ultrasonic-based method, recently developed by the authors. The numerical simulation of the resin infusion process involved the modeling of the resin flow through the reinforcement, the heat exchange in the part and within the mold, and the crosslinking reaction of the resin. The time necessary to fill the component has been measured by an optical fiber-based equipment and compared with the simulation results.

Different hybrid epoxy formulations were produced and cold-cured, monitoring the properties development during low temperature curing and aging. All systems were based on silane functionalized bis-phenol A (DGEBA) resins (Part A), cured at ambient temperature with two amine hardeners (Part B). The different components of the formulations were selected on their potential capability to bring about enhancements in the glass transition temperature. The durability of the produced hybrids was probed in comparison to the corresponding neat epoxies by monitoring changes in glass transition temperature (Tg) and flexural mechanical properties after exposure to different levels of humidity and immersion in water and at temperatures slightly higher than the local ambient temperature, in order to simulate the conditions encountered during summer seasons in very humid environments. The thermal degradation resistance of the hybrid systems was also evaluated by thermogravimetric analysis.

In this research, a simple experimental apparatus based on a bipolar electrode (BPE) configuration was set up, in order to tackle erosion-corrosion problems of materials of interest in the oil and gas field. As a case study, the resistance to erosion and corrosion of carbon steel samples coated by Electroless Nickel Plating and by thermo-sprayed coating with the high velocity oxy fuel (HVOF) process was investigated. The main objective was to demonstrate if this simple, contactless technique could be applied to effectively discriminate the erosion-corrosion behavior of different materials in a vast range of experimental conditions. In fact, by means of polarization curves, visual inspection and morphological analysis by scanning electron microscope (SEM), the effects due to erosion-corrosion by solid particles, by fluid and those due to simple erosion were evaluated.

Out-of-plane permeability of reinforcement preforms is of crucial importance in the infusion of large and thick composite panels, but so far, there are no standard experimental methods for its determination. In this work, an experimental set-up for the measurement of unsaturated through thickness permeability based on the ultrasonic wave propagation in pulse echo mode is presented. A single ultrasonic transducer, working both as emitter and receiver of ultrasonic waves, was used to monitor the through thickness flow front during a vacuum assisted resin infusion experiment. The set-up was tested on three thick carbon fiber preforms, obtained by stacking thermal bonding of balanced or unidirectional plies either by automated fiber placement either by hand lay-up of unidirectional plies. The ultrasonic data were used to calculate unsaturated out-of-plane permeability using Darcy&rsquo, s law. The permeability results were compared with saturated out-of-plane permeability, determined by a traditional gravimetric method, and validated by some analytical models. The results demonstrated the feasibility and potential of the proposed set-up for permeability measurements thanks to its noninvasive character and the one-side access.

Fish industry waste is attracting growing interest for the production of environmentally friendly materials for several different applications, due to the potential for reduced environmental impact and increased socioeconomic benefits. Recently, the application of fish industry waste for the synthesis of value-added materials and energy storage systems represents a feasible route to strengthen the overall sustainability of energy storage product lines. This review focused on an in-depth outlook on the advances in fish byproduct-derived materials for energy storage devices, including lithium-ion batteries (LIBs), sodium-ion (NIBs) batteries, lithium-sulfur batteries (LSBs), supercapacitors and protein batteries. For each of these, the latest applications were presented together with approaches to improve the electrochemical performance of the obtained materials. By analyzing the recent literature on this topic, this review aimed to contribute to further advances in the sustainability of energy storage devices.

Continuous induction welding for thermoplastic matrix composites requires an accurate modeling of the temperature distribution in the laminates, depending on the electromagnetic field. In this work, a transient three-dimensional finite element (FE) model was developed in order to study the heat transfer phenomena, and melting and crystallization in the welding area during the continuous induction welding of carbon fiber reinforced Poly(ether ether ketone) (CF/PEEK) laminates. The multiphysics problem was solved by coupling electromagnetic and heat transfer equations considering matrix melting and crystallization behavior. The model was able to simulate the continuous process along a linear path at a constant speed. The computed temperatures were in good agreement with experimental measurements. Several numerical simulation were used for selecting a processing window as a function of coil speed and current, for the welding of CF/PEEK joints. The results of welding experiments were evaluated by single lap shear tests and morphology characterization of the welded interfaces and fracture surfaces. Keywords: Carbon fiber, Finite element analysis, Joining, Heat treatment, Induction welding, Thermoplastic resin

During autoclave processing of composites for high-performance applications, it is mandatory to limit the porosities, which mainly depend on the hydrostatic pressure in the resin. This pressure, which is not constant during heating being affected either by resin flow either by elastic stress in the fiber stack, can be significantly different from the autoclave pressure. Modeling of resin flow and stress in the fiber stack is a key issue for prediction of the resin hydrostatic pressure, which can be related to void development. Also, the viscosity of the thermosetting matrix is a relevant parameter since it is not constant but evolves during curing going through a minimum and then increasing to an infinite value at gel point. In this work, a viscoelastic model is adopted to calculate the evolution of resin pressure during an autoclave cycle up to gelation, accounting for viscosity and degree of reaction changes. Therefore, the model includes a kinetic and rheological model whose input parameters have been experimentally determined by Differential Scanning Calorimetry and rheological analysis. The predicted resin pressure for three case studies associated to different composite and bleeder thicknesses and reinforcement materials have been discussed. POLYM. ENG. SCI., 57:631–637, 2017. © 2017 Society of Plastics Engineers

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The anisotropy of a short fiber reinforced composite produced by injection molding of basalt fibers and polypropylene matrix has been studied by X-ray microtomography (or micro-CT). Fiber orientation was analyzed using four stereological methods: Mean Intercept Length (MIL), Volume Orientation (VO), Star Volume Distribution (SVD) and Star Length Distribution (SLD). The fabric tensor obtained from micro-CT analysis provided information on the fiber orientation, indicating that fibers were partially aligned in the injection direction.

In this work the architectural anisotropy of short fiber reinforced polymers (SFRPs) has been characterized using X-ray computed micro-tomography (micro-CT) with four different morphometric methods: Mean Intercept Length (MIL), Volume Orientation (VO), Star Length Distribution (SLD) and Star Volume Distribution (SVD). The fabric tensor obtained from micro-CT analysis provided information on the fiber orientation, indicating that fibers were partially aligned in the injection direction. The fiber length and orientation obtained from optical microscopy and from the morphometric analysis in 3D, respectively, has been used to determine the mechanical properties of the composite sample, using a model based on micro and macromechanics. This approach leads to the prediction of the elastic constants of the component for any possible composite morphology resulting from injection, representing a key need for the design of SFRP components.

The mechanical and electrochemical behavior of ultrasonic spot welded hybrid joints, made of AA5754 aluminum and carbon fiber reinforced epoxy with a co-cured thermoplastic surface layer, was studied. The effect of the welding parameters (energy and force) and the thickness of a thermoplastic film, applied as an upper ply in the composite lay-up, on the development of adhesion strength, was investigated. The best mechanical results were obtained when the welding parameters were able to achieve a large bonding area of mechanical interlocking between naked carbon fibers and aluminum and a better load distribution. The electrochemical results excluded the possibility of galvanic corrosion between aluminum and composite adherends thanks to the insulating action provided by the thermoplastic film.

Stress relaxation behavior of unidirectional AS4/8852 carbon/epoxy composites at high temperatures has been investigated. Specimens with an off axis angle of 90° and ±45° have been exposed to constant strain and high temperature. The mechanical results have been modeled by Standard Linear Solid model. The obtained parameters have been implemented in a finite element (FEM) model able to predict the residual stresses in carbon fiber reinforced composites, both in the elastic and in the viscoelastic field.Stress relaxation behavior of unidirectional AS4/8852 carbon/epoxy composites at high temperatures has been investigated. Specimens with an off axis angle of 90° and ±45° have been exposed to constant strain and high temperature. The mechanical results have been modeled by Standard Linear Solid model. The obtained parameters have been implemented in a finite element (FEM) model able to predict the residual stresses in carbon fiber reinforced composites, both in the elastic and in the viscoelastic field.

The approach for joining thermosetting matrix composites (TSCs) proposed in this study is based on the use of a low melting co-cured thermoplastic film, added as a last ply in the stacking sequence of the composite laminate. During curing, the thermoplastic film partially penetrates in the first layer of the thermosetting composite, leading to macro-mechanical interlocking as the main connection mechanism between the thermoplastic film and the underlying composite. After curing, the thermosetting composite joints with the thermoplastic modified surface can be assembled by welding. Welding of the TSC-TSC joints is performed by ultrasonic and induction welding. The weld strength is investigated by morphological characterization of cross sections and failure surfaces and by mechanical testing. The effect of the thermoplastic film thickness on the welding process and on its outcome is also analyzed. Both induction and ultrasonic welding mostly result in good-quality welded joints. The welding process used as well as the initial thickness of the thermoplastic film are found to have a significant effect on the final thickness of the weld line and on the location of failure. Thicker thermoplastic films are found to ease the welding processes.

A deep eutectic solvent (DES) based on choline chloride and urea (ChCl-U) was used to prepare epoxy compositions based on low molecular weight diglycidyl ether of bisphenol A (DGEBA) resin. Fourier transform infrared (FTIR) spectroscopy, rheometry and differential scanning calorimetry (DSC) were, then, used to investigate the curing mechanism of epoxy mixtures as a function of the DES content. The results confirmed that the eutectic mixture of choline chloride and urea was able to initiate the reaction of chain homopolymerization in the absence of the hardener, thus acting as a biodegradable and sustainable catalytic curing agent for epoxy resins. Nonisothermal reaction kinetics was modeled with the results obtained by ICTAC Kinetic Project confirming the role of the analyzed deep eutectic solvent in accelerating the homopolymerization of epoxy groups.

The engineering aspects, which are associated with the development of nanocomposites, involve in either final properties or processability of nanocomposites. Both are affected by the distribution of nanofiller in the matrix and by the aspect ratio of the nanofiller. A nanofilled thermosetting resin can be exploited as a matrix for continuous fibers when the alignment of a high aspect ratio nanofiller is achieved, and in this case, a hierarchical composite is obtained. In this study, a new procedure for the alignment of nanofillers in a thermosetting matrix is proposed. The two-step approach is based on (i) the alignment of nanofillers (carbon nanotubes, graphene, etc.) in thermoplastic fibers by a fiber spinning process and (ii) the use of these nanocomposite fibers as a carrier to bring aligned nanofillers into a reactive thermosetting resin. These fibers, soluble in the thermosetting resin, release the nanofillers orientated according to the direction in which fibers are positioned, even after the curing of the matrix. The proof of concept is demonstrated by producing melt spun polyethylene terephtalate (PETg) fibers filled with graphene nanoplatelets (GNP) and multiwall carbon nanotubes (MWCNT) with a very high filler content (up to 10 wt%) in view of producing a hierarchical composite. POLYM. COMPOS., 36:1096–1103, 2015. © 2015 Society of Plastics Engineers

The growing use of reinforcement preforms during composite manufacturing requires resin soluble binders which significantly affect the properties of crosslinking thermosetting resins. In this study, for the first time the influence of an epoxy preforming binder on the curing kinetics and chemorheological behavior of a crosslinking epoxy matrix was studied. The results proved that the addition of the binder lead to a significant change of the curing behavior suggesting that the epoxy binder was an essential component needed to complete the stoichiometry of the resin-hardener mixture. The developed kinetic and chemorheological model of the experimental results could be used for process optimization.

Ultrasonic metal welding has been applied for joining aluminum AA5754 sheets to a thermoset matrix composite consisting in a carbon fiber reinforced epoxy resin (CF/epoxy). To overcome the limitations of thermosetting resins, that, unlike thermoplastic polymers, cannot melt due to their chemical structure, a thermoplastic film of Polyamide 6 (PA6) has been used as a surface layer of the CF/epoxy stack before curing. The functional surface created on the thermoset matrix composite enables a fast welding with a metallic sheet. By a proper selection of welding energy and force, an average adhesion strength of 34.8 MPa has been obtained on CF/epoxy-PA6-AA5754 ultrasonically welded joints. The morphological characterization has revealed that the aluminum-composite interface is characterized by carbon fibers in a direct contact or even embedded in aluminum, whose surface presents pores and crevices due to the pronounced plastic deformation of the Al interfacial area.

Waterlogged wood samples of Ulmus sp. and Fraxinus sp. from the ancient harbor of Otranto in Southern Italy were radiocarbon dated by accelerator mass spectrometry (AMS) and examined for physical and chemical changes to assess the degree of degradation. The analyzed woods were dated to the 2nd half of the twelfth – 1st half of the thirteenth centuries AD. The results of all the used methods (maximum water content, basic density, shrinkage, XRD analysis and holocellulose content) indicated a low level of degradation in the inner part of the wooden find. The outer and middle part, on the other hand, showed a greater degradation level. An important result is the identification of a not homogeneous degradation in the different parts of the examined wooden block, which will affect the design of the consolidating treatment.

The development of improved cold-cured resins, to be used as either adhesives or matrices for FRP (fiber reinforced polymer) composites employed in the construction industry, has become the focus of several academic and industrial research projects. It is expected that the use of nano-structured organic&ndash, inorganic hybrid materials could represent a realistic alternative to commercial epoxy-based resins due to their superior properties, especially in terms of higher durability against: moisture, temperatures, harsh environments, and fire. In this context, organic&ndash, inorganic epoxy hybrids were synthesized by a modified sol&ndash, gel method without the addition of water. The experimental formulations were prepared starting from a mixture of a silane-functionalized epoxy resin, alkoxysilane components and a deep eutectic solvent (DES) based on a blend of choline chloride and urea. The latter was added in two different loads in order to analyze in depth its effect as a promoter for an effective dispersion of silica nano-phases, formed through hydrolysis and condensation reactions, into the cross-linked epoxy network. The produced formulations were cold-cured for different time spans in the presence of two hardeners, both suitable for a curing process at ambient temperature. In this first part of a wider experimental program, several analyses were carried out on the liquid (rheological and calorimetric) and cold-cured (calorimetric, thermogravimetric, dynamic-mechanical, flexural mechanical, and morphological) systems to evaluate and quantify the improvement in properties brought about by the presence of two different phases (organic and inorganic) in the same epoxy-based hybrid system.