The extensive production and use of fossil-based plastics have led to their ubiquity worldwide, causing growing concern and environmental problems. Consequently, developing biobased polymers and biobased composite materials, aligned with circular economy principles, is now the focus as a sustainable alternative to fossil-based plastics. This work aimed to develop and characterise a new, fully biobased, and biodegradable material composite with properties similar to traditional fossil-based plastics, allowing its use in cosmetic product applications as an alternative to commonly used fossil-based plastics. A novel biobased composite comprising poly(3-hydroxybutyrate-co-3-hydroxyvalerate (PHBV), polylactic acid (PLA) chitosan (CS), acetyl tributyl citrate (ATBC) plant essential oils, and phycocyanin was successfully developed and processed using various techniques confirming its processability and versatility. Characterisation of the developed composites showed a reduction in mechanical properties with the addition of ATBC, essential oil and phycocyanin, with tensile results within the typical behaviour for PP (polypropylene) and PE (polyethylene). The thermal properties of the developed composites showed working temperatures in the same range as PP and PE. The results obtained are promising and, to the best of our knowledge, this work presents the first green material composite comprising PHBV, PLA, CS, essential oil, ATBC, and phycocyanin specifically designed for cosmetic packaging as a sustainable alternative to fossil-based plastics.

Injection moulding is a very popular technology for shaping plastics. Its history stretches back to the nineteenth century, and, as a consequence, it has developed outside the framework of digitisation. In order to fully implement the concepts of Industry 4.0, we need to update these legacy technologies so that they can fully benefit from the developments inherent in the “Internet of Things” and allow the process of injection moulding to take full advantage of digital optimisation so that it can fit effectively in the digital factory. In this work, we explore the quantitative use of X-ray scattering as a technology that can provide dynamic and multiscale feedback during the injection moulding cycle to be able to exploit digital twin technology as a means to optimise the operational parameters involved in injection moulding and to enable digital design of moulds in the fullest sense. This manuscript provides a way to mark future work and draw these possibilities to a wider audience.

Side-chain liquid crystal polymers have been mixed with ferromagnetic particles, and the formation of a monodomain in magnetic fields studied. At relatively low concentrations, the presence of ferroparticles substantially speeds up the rate of formation of a monodomain within the magnetic field, and, at a given concentration of ferroparticles, that rate is independent of the magnetic field’s strength. In this way, the rapid formation of a monodomain is possible at magnetic field strengths far lower those required for the liquid crystal polymer alone. This is anticipated to be very helpful in the fabrication of devices based on monodomain liquid crystal elastomers. Wide-angle x-ray scattering has been used to monitor the formation of the monodomain and small-angle x-ray scattering gives some indication of the ferroparticles’ behaviour. A model is developed to explain their behaviour. The alignment properties of the ferroparticles are related to their ability to form chains under the influence of very low magnetic fields; these chains are of relatively low stability and may become disrupted after long periods of time, high magnetic fields, or high concentrations. In general, the best results for alignment were at volume fractions below 1%, and under these conditions there is the potential for producing monodomain samples with improved properties; in particular, shape changes with temperature are significantly larger as a result of improved backbone orientation. Experiments involving monodomain formation and director realignment suggest that the presence of ferroparticles results in a modification of the mechanism for alignment development, driven by the organization of the polymer backbone, as a consequence of the constraints offered by the morphology of the chains of the ferroparticles.

This research aims to check the chargeability of sodium hypochlorite and the efficacy evaluation of an airassisted electrostatic disinfection device. Five different inanimate surfaces i.e., wood, glass, stainless steel, plastic and fabric were considered to examine the performance in terms of efficacy, survival time, off-target losses, spray coverage and the volume of disinfectant consumed. A significant charge-to-mass level of 2.43 mC/kg was achieved for sodium hypochlorite at an applied voltage of 2.0 kV, a liquid flowrate of 253 ml/min and applied air pressure of 4.0 bar. The experimental results found that 1000 mg/L of sodium hypochlorite concentration effectively eliminated Pseudomonas aeruginosa, Clostridium perfringens and Bacteriophage MS2 colonies.

We recently introduced the possibility of performing operando small-angle X-ray scattering measurements using a novel industrially relevant injection moulding system for plastics. We show that useful time-resolving measurements can be performed with a time-cycle of 1 s and highlight the possible steps to reduce this to 0.5 s. We show how we can use the transmission measurements to provide a time marker when plastic first enters the mould cavity in the region probed by the incident X-ray beam. We show the opportunities provided by this experimental stage mounted on the NCD-SWEET beamline at ALBA to probe the reproducibility of the injection moulding system on different scales. The design of the equipment allowed for the development of the structure and the morphology to be evaluated in different parts of mould cavity, and we evaluated any differences in a rectangular mould cavity. We identified future prospects for this equipment in terms of novel mould heating and cooling systems and the opportunities for quantitatively evaluating radical approaches to injection moulding technology.

The pace of transition from prototyping to rapid manufacturing within the framework of Industry 4.0 has greatly increased. This increased rate of use of direct digital manufacturing to produce commercial products takes place within the backdrop of the major societal challenge of climate change. There is now an increased realization of the need to make wider use of sustainable materials in the manufacturing of products with a much -reduced carbon foot print.

Rhododendron ponticum is an invasive species that spreads rapidly and is described as one of the biggest threats to peatlands in Ireland. This study offers an innovative approach to utilizing Rhododendron waste. Initially, sawdust was submitted to a bleaching treatment and the nanofibrillated cellulose (NFC) was obtained using two different methods: ultra-fine friction grinding and twin-screw extrusion with the assistance of TEMPO (2,2,6,6-tetramethyl-1-piperidinyloxy) pre-treatment. The samples processed through twin-screw extrusion exhibited the presence of NFC at five intervals, as confirmed by TEM analysis. However, these samples displayed a higher diameter deviation compared to those processed through grinding alone. Notably, after 20 extrusion steps, the NFC diameter became more uniform, reaching approximately 35 nm. Sedimentation tests showed that extrusion produced more homogeneous cellulose size than the grinder method. However, FTIR characterization for the samples showed a unique band related to C-O-C glycosidic linkage. The results showed that grinding breaks these groups resulting in crystallinity values lower than extrusion, 50 % compared 60 %. Therefore, NFC with 20 steps by grinding was blended with polycaprolactone to produce a 3D scaffold using a 3D printer at different ratios of 1-5 % addition. The effect of 1 % of NFC was unique showing significant enhanced mechanical properties compared to pure polycaprolactone (PCL), additionally, the NFC does not exhibit toxicity so these materials show promise for biomedical applications.

In this study, we describe the design and fabrication of an industrial injection moulding system that can be mounted and used on the NCD-SWEET small-angle X-ray scattering beamline at ALBA. We show how highly useful time-resolved data can be obtained using this system. We are able to evaluate the fraction of the material in the mould cavity and identify the first material to solidify and how this varies with the injection temperature. The design follows current industrial practice and provides opportunities to collect time-resolved data at several points within the mould cavity so that we can build up a 4D perspective of the morphology and its temporal development. The quantitative data obtained will prove invaluable for the optimisation of the next generation of injection moulding techniques. This preliminary work used results from the injection moulding of a general-purpose isotactic polypropylene.

1 Centre for Rapid and Sustainable Product Development, Polytechnic of Leiria, 2430-080 Marinha Grande, Portugal; daniel.p.silva@ipleirira.pt (D.S.); joao.pinheiro@ipleiria.ptm (J.P.); saba.abdulghani@nms.unl.pt (S.A.); paula.faria@ipleiria.pt (P.P.-F.); artur.mateus@ipleiria.pt (A.M.) 2 NCD-SWEET Beamline, Alba Synchrotron Light Source, Cerdanyola del Vallès, 08290 Barcelona, Spain; ckamma@ansto.gov.au (C.S.K.-L.); esolano@cells.es (E.S.); guilmar@cells.es (J.C.M.) * Correspondence: geoffrey.mitchell@ipleiria.pt; Tel.: +351-962-426-925 † Presented at the Materiais 2022, Marinha Grande, Portugal, 10–13 April 2022.

28 Codium tomentosum hydroethanolic extract was obtained using a pilot solid-liquid 29 extractor to validate the anti-browning functionality of the extract under industrial 30 conditions. Fresh-cut apple slices were coated by immersion in: 1) a seaweed extract 31 solution (0.5 % w/v) and 2) a commercial coating, and the two sets of samples were 32 compared with a control (immersion in water). Packaged samples were stored, under 33 ambient and modified atmosphere conditions at 4˚C. After 30 days of storage, the 34 samples which were coated with the seaweed extract and packaged under modified 35 atmosphere, demonstrated lower peroxidase activity and polyphenol oxidation when 36 compared with the samples treated with the commercial additive. These results confirm, 37 at pilot scale and under industrial production conditions, the efficacy of the seaweed 38 extract as a bio-based substitute for the synthetic coatings which are currently used to 39 prevent browning in fresh-cut apples. 40

Rocha is a Portuguese pear cultivar with high economic importance in the Portuguese Western Region. Degradative processes following its manipulation can quickly lead to product rejection, especially when sold as a freshcut product. The efficacy of a marine-based edible coating to inhibit superficial browning development in freshcut Rocha pear slices was investigated over a storage period of 15 days. The aqueous extract of Codium tomentosum, an edible green seaweed, was incorporated in an edible coating (0.5 g 100 mL(-1)) for fresh-cut Rocha pear. This novel treatment effect on the quality parameters of the pears was compared with a commercial coating currently used by industry and a control (dipping in deionised water). After 15 days storage at 4 degrees C, samples treated with the seaweed extract exhibited fewer colour changes and lower rates of superficial browning than control and commercial samples. Seaweed extract treatment was also observed to inhibit yeast and mould development, which may further contribute to shelf-life extension.

Understanding the mechano–biological coupling mechanisms of biomaterials for tissue engineering is of major importance to assure proper scaffold performance in situ. Therefore, it is of paramount importance to establish correlations between biomaterials, their processing conditions, and their mechanical behaviour, as well as their biological performance. With this work, it was possible to infer a correlation between the addition of graphene nanoparticles (GPN) in a concentration of 0.25, 0.5, and 0.75% (w/w) (GPN0.25, GPN0.5, and GPN0.75, respectively) in three-dimensional poly(ε-caprolactone) (PCL)-based scaffolds, the extrusion-based processing parameters, and the lamellar crystal orientation through small-angle X-ray scattering experiments of extruded samples of PCL and PCL/GPN. Results revealed a significant impact on the scaffold’s mechanical properties to a maximum of 0.5% of GPN content, with a significant improvement in the compressive modulus of 59 MPa to 93 MPa. In vitro cell culture experiments showed the scaffold’s ability to support the adhesion and proliferation of L929 fibroblasts (fold increase of 28, 22, 23, and 13 at day 13 (in relation to day 1) for PCL, GPN0.25, GPN0.5, and GPN0.75, respectively) and bone marrow mesenchymal stem/stromal cells (seven-fold increase for all sample groups at day 21 in relation to day 1). Moreover, the cells maintained high viability, regular morphology, and migration capacity in all the different experimental groups, assuring the potential of PCL/GPN scaffolds for tissue engineering (TE) applications.

Understanding biaxial deformation is essential for a more realistic evaluation of rubber elasticity compared to the more usual uniaxial deformation. To study crystallisation occurring during biaxial deformation of natural rubber films, a new simple equipment has been designed and assembled. The equipment, mounted in the beamline of ALBA synchrotron light source facility, allowed the in-situ measurement of X-ray scattering of natural rubber during biaxial deformation. This work provides, for the first time, quantitative information on crystallisation during biaxial extension.

This article aims to study a new ceramic paste mixing red clay with coffee residues in 3D printing, proposing an effective solution for the recycling of coffee residues. Intense studies were made on clay paste containing 5, 10, 15, and 20% coffee grounds. The morphological and chemical aspects were evaluated through SEM, Micro CT, and FTIR images; physical and mechanical properties were assessed by mechanical resistance, absorption, and drying tests, with the aim to obtain results on the hardness, permeability, absorption, and weight; finally, 3D-printing tests were performed to study the paste behavior and understand its advantages in new emerging technologies. The incorporation of coffee residues in red clay results in a light and very porous product; thus increasing the water absorption and apparent porosity. Some pieces were created to test the structural capacity and consistency of the paste. The idea was to create bricks, floors, and coverings.

Injection moulding is the most common fabrication technology used to shape plastics [...]

This work focuses on understanding the action of a novel seaweed extract with anti-browning functionality in fresh-cut apples. Organic fresh-cut apples were coated by immersion in an aqueous Codium tomentosum seaweed extract (0.5 % w/v), packaged under ambient atmospheric conditions in plastic bags, and stored at 4 ˚C for 15 days. Browning-related enzymatic activities, as well as targeted gene expression related to superficial browning, were monitored immediately after coating and followed at five-day intervals, until a final storage period of 15 days. Gene expression was particularly affected one hour after coating application (day 0), with no expression registered for peroxidase (mdPOD) and phenylalanine ammonia-lyase (mdPAL) genes in the coated samples. A reduction in polyphenol oxidase expression levels was also observed. After 15 days of storage, the coated samples developed lower browning levels and presented distinctly lower activities of polyphenol oxidase and peroxidase - the oxidative enzymes predominantly involved in enzymatic browning. The observed post-coating suppression of mdPAL and mdPOD expression, and reduction in mdPPO expression, suggest that the seaweed C. tomentosum extract delays the activation of these genes, and decreases enzymatic activity, which in turn accounts for the coating’s anti-browning effect.

Liquid crystal polymers, through covalent bonding, combine the spontaneous long range orientational order of the liquid crystal state with the entropically driven random coil configurations of the skeletal polymer chains in a single material [...]

Direct digital manufacturing consists of a set of techniques that enable products to be fabricated directly from their digital definition, without the use of complex tooling or moulds. This manufacturing approach streamlines prototyping and small-scale production, as well as the mass customization of parts with complex designs immediately fixed before fabrication. With broad applicability, there are clearly opportunities in the field of medical devices for its use. However, many of the developments of direct digital manufacturing focus on simply specifying the shape or the form of the product, and this limited scope throws away many of the particular advantages of direct digital manufacturing. This work is focused on remedying this situation so that the digital specification of the fabricated product includes the properties as well as the form of the product. We use in situ time-resolving small-angle X-ray scattering measurements performed at the ALBA Synchrotron Light Source in Barcelona to evaluate the control that can be exerted on the morphology of a semi-crystalline polymer during extruder-based 3D printing. We use this as a methodology for printing the patterns of the morphology of the polymer to realise the patterns of properties of the polymeric material, specifically the modulus of the polymer. We give an example of products produced in this manner that contain spatial variation in their properties.

The melting/crystallization properties of blends obtained by mixing two isotactic polypropylene (iPP) samples synthesized using single-site metallocene catalyst systems and containing a high and low concentration of rr triads as stereo-defects, are studied. The changes occurring at lamellar length scale during a heating/cooling cycle at constant scanning rate are followed in situ by performing time-resolved small angle X-ray scattering (SAXS) measurements. Data analysis demonstrates that the evolution of the SAXS intensity with increase/decrease of the temperature is controlled by the separate melting/crystallization of the two components, the differences in the thermal expansion (contraction) coefficient of the amorphous and crystalline phases and the role of thermal fluctuations in electron density. The two components give rise to different populations of intermixed lamellar stacks in the blends which originate from the good miscibility of the low and high stereoregular samples in the melt.

Antioxidant activity is an important feature for food contact materials such as packaging, aiming to preserve freshness and retard food spoilage. Common bioactive agents are highly susceptible to various forms of degradation; therefore, protection is required to maintain functionality and bioavailability. Poly(ε-caprolactone) (PCL), a biodegradable GRAS labeled polymer, was used in this study for encapsulation of α-tocopherol antioxidant, a major component of vitamin E, in the form of electrospun fibers. Rheological properties of the fiber forming solutions, which determine the electrospinning behavior, were correlated with the properties of electrospun fibers, e.g., morphology and surface properties. Interactions through hydrogen bonds were evidenced between the two components. These have strong effect on structuration of macromolecular chains, especially at low α-tocopherol amounts, decreasing viscosity and elastic modulus. Intra-molecular interactions in PCL strengthen at high α-tocopherol amounts due to decreased solvation, allowing good structural recovery after cease of mechanical stress. Morphologically homogeneous electrospun fibers were obtained, with ~6 μm average diameter. The obtained fibers were highly hydrophobic, with fast release in 95% ethanol as alternative simulant for fatty foods. This induced good in vitro antioxidant activity and significant in vivo reduction of microbial growth on cheese, as determined by respirometry. Therefore, the electrospun fibers from PCL entrapping α-tocopherol as bioactive agent showed potential use in food packaging materials.