The purpose of this paper is to propose a methodology to optimise the granular skeleton assembly of cementitious materials containing non-spherical aggregates. The method is general and can be applied to any granular skeleton whatever the aggregate shape, size, or composition because it is simply based on the direct minimisation of the inter- granular porosity to consequently increase the skeleton’s compactness. Based on an experimental design approach, this method was applied to and validated for bio-based oyster shell (OS) mortar with 100% aggregate replacement. First, the best combination of seven crushed oyster shell particle classes was determined and compared with a stan- dardised sand skeleton (0/4 mm) and three other non-optimised OS gradings in terms of intergranular porosity. In particular, it is shown that simply mimicking a reference grading curve initially designed for spherical particles with non-spherical particles led to poor performances. Then, different mortars were cast with the standardised sand skele- ton, the optimised OS grading, and the three other non-optimised OS gradings by keeping the water-to-cement ratio (0.5), the aggregate bulk volume, and the cement paste content constant. Mechanical tests in compression confirmed the higher performance of the optimised OS mortar, validating the global optimisation approach. However, the high elongation of the oyster shell aggregates led to high skeleton intergranular porosities -- even after optimisation -- and the cement paste content needed to be adapted. For a given granular skeleton and for a constant aggregate bulk vol- ume, the increase of the cement paste content led to an increase of both the filling ratio and the mechanical properties (compressive and flexural strengths). Finally, it is shown that the proposed skeleton optimisation and a cement paste content adjustment allowed recovering good mechanical properties for an oyster shell mortar with 100% aggregate replacement, especially in flexural tension.

The growing concern over water pollution and waste management requires innovative solutions that promote resource efficiency within a circular economy. This study aims to utilize rice husk (RH) as a sustainable feedstock to develop highly porous silica particles and generate valuable by-products, addressing the dual challenges of waste reduction and water contamination. We hypothesize that optimizing the production of amorphous silica from acid-washed RH will enhance its adsorptive properties and facilitate the concurrent generation of bio-oil and syngas. Amorphous silica particles were extracted from acid-washed RH with a yield of 15 wt% using a combination of acid washing at 100 °C, pyrolysis at 500 °C, and calcination at 700 °C with controlled heating at 2 °C/min. The optimized material (RH2-SiO2), composed of small (60–200 nm) and large (50–200 µm) particles, had a specific surface area of 320 m2/g, with funnel-shaped pores with diameters from 17 nm to 4 nm and showed a maximum cadmium adsorption capacity of 407 mg Cd/g SiO2. Additionally, the pyrolysis process yielded CO-rich syngas and bio-oil with an elevated phenolic content, demonstrating a higher bio-oil yield and reduced gas production compared to untreated RH. Some limitations were identified, including the need for bio-oil upgrading, further research into the application of RH2-SiO2 for wastewater treatment, and the scaling-up of adsorbent production. Despite the challenges, these results contribute to the development of a promising adsorbent for water pollution control while enhancing the value of agricultural waste and moving closer to a circular economy model.

Avec le soutien d’une unité du CNRS de Montpellier, une équipe de recherche de l’Université de Pau et des Pays de l’Adour (UPPA) s’intéresse à la valorisation de la balle de riz, la cosse qui entoure ces petits grains bien connus. Leurs objectifs? Récupérer bio-huile et silice, deux super ingrédients présents dans ce déchet, qui pourraient servir de biocarburant ou encore d’agent décontaminant de l’eau.

In contrast to man-made materials, nature can produce materials with remarkable mechanical properties from relatively weak constituents. Nacre from seashells is a compelling example: despite being comprised mostly of a fragile ceramic (polygonal calcium carbonate tablets), it exhibits surprisingly high levels of strength and toughness. This performance is the result of an elegant hierarchical microstructure containing a small volume fraction of biopolymers at interfaces. The product is a composite material that is stiff and hard yet surprisingly tough, an essential requirement to protect the seashell from predators. Building a comprehensive understanding of the multi-scale mechanisms that enable this performance represents a critical step toward realizing strong and tough bio-inspired materials. This paper details a nanoscale experimental investigation into the toughening mechanisms in natural nacre and presents a way to translate this understanding to the design of new bioinspired composites. In situ three point bending fracture tests are performed to identify and quantify the toughening mechanisms involved during the fracture of natural nacre at the nanoscale. At the macro and micro scales, previous fracture tests [1] and [2] performed in situ enabled observation of spreading of damage outward from the crack tip. In this study, fracture tests are performed in situ an atomic force microscope to link the larger-scale damage spreading to sliding within the tablet-based microstructure. To quantify the magnitude of sliding and its distribution, images from the in situ AFM fracture tests are analyzed using standard and new algorithms based on digital image correlation techniques which allow for discontinuous displacement fields. Ultimately, this comprehensive methodology provides a framework for broad experimental investigations into the failure mechanisms of bio- and bio-inspired materials.

Natural materials (e.g. nacre, bone, and spider silk) exhibit unique and outstanding mechanical properties. This performance is due to highly evolved hierarchical designs. Building a comprehensive understanding of the multi-scale mechanisms that enable this performance represents a critical step toward realizing strong and tough bio-inspired materials. This paper details a multi-scale experimental investigation into the toughening mechanisms in natural nacre. By applying extended digital image correlation and other image processing techniques, quantitative information is extracted from otherwise prodominantly qualitative experiments. In situ three point bending fracture tests are performed to identify and quantify the toughening mechanisms involved during the fracture of natural nacre across multiple length scales. At the macro and micro scales, fracture tests performed in situ with a macro lens and optical microscope enable observation of spreading of damage outward from the crack tip. This spreading is quantified using an iso-contour technique to assess material toughness. At the nanoscale, fracture tests are performed in situ an atomic force microscope to link the larger-scale damage spreading to sliding within the tablet-based microstructure. To quantify the magnitude of sliding and its distribution, images from the in situ AFM fracture tests are analyzed using new algorithms based on digital image correlation techniques which allow for discontinuous displacement fields. Ultimately, this comprehensive methodology provides a framework for broad experimental investigations into the failure mechanisms of bio- and bio-inspired materials.

Nacre, the iridescent material in seashells, is one of many natural materials employing hierarchical structures to achieve high strength and toughness from relatively weak constituents. Incorporating these structures into composites is appealing as conventional engineering materials often sacrifice strength to improve toughness. Researchers hypothesize that nacre's toughness originates within its brick-and-mortar-like microstructure. Under loading, bricks slide relative to each other, propagating inelastic deformation over millimeter length scales. This leads to orders-of-magnitude increase in toughness. Here, we use in situ atomic force microscopy fracture experiments and digital image correlation to quantitatively prove that brick morphology (waviness) leads to transverse dilation and subsequent interfacial hardening during sliding, a previously hypothesized dominant toughening mechanism in nacre. By replicating this mechanism in a scaled-up model synthetic material, we find that it indeed leads to major improvements in energy dissipation. Ultimately, lessons from this investigation may be key to realizing the immense potential of widely pursued nanocomposites.