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  • Thermally modified wood: assessing the impact of weathering on mechanical strength and exposure to subterranean termites
    Publication . Godinho, Delfina; Lourenco, Ana; Araújo, Solange; Machado, José Saporiti; Nunes, Lina; Duarte, Marta; Duarte, Sónia; Ferreira, Cristina; Quilhó, Teresa; Cunha Diamantino, Teresa; Gominho, Jorge
    ABSTRACT: The main objective of this study was to evaluate the mechanical properties of three thermal-modified wood species when exposed to weathering in urban and maritime/industrial environments and their durability against subterranean termites. The wood species studied were Maritime pine, ash, and blackwood acacia. All wood samples were exposed to two different environments (urban and maritime/industrial) for 24 months. Then, its physical and mechanical properties were evaluated (modulus of elasticity (MOE), modulus of rupture (MOR), compression strength (CS), and modulus of compression (MOC). Thermally modified woods revealed a lower density, which could explain the loss of MOE and MOR. In compression, no significant changes were verified. The weathered samples showed changes in mechanical properties, mostly verified in MOE and MOR, where some decreases were reported in both locations. Tests were performed to evaluate biodegradation and the resistance of all wood samples to subterranean termites. The grade of attack (approximate to 4) and termite survival rate were similar in all wood species (above 75% and lower than 80%), except for modified acacia (59%), which could indicate that thermal modification increased toxic substances. The cellulose degradation was reflected in FTIR-ATR and Py-GC/MS in natural and thermally modified woods. Py-GC/MS showed a decrease in levoglucosan, while lignin suffered some modifications with slight changes in monomeric composition reflected by the reduction of the S/G ratio. No changes were found between the two environments, and thermal modification did not give extra protection against termites and weathering.
  • Thermoelectric Properties of Tetrahedrites Produced from Mixtures of Natural and Synthetic Materials
    Publication . Santos, Beatriz; Esperto, Luís; Figueira Vasques, Isabel; Mascarenhas, João; Lopes, E.B.; Salgueiro, Rute; Silva, Teresa; Correia, Jose B.; de Oliveira, Daniel Pipa Soares; Pereira Gonçalves, Antonio; Neves, Filipe
    ABSTRACT: Thermoelectric materials have considerable potential in the mitigation of the global energy crisis, through their ability to convert heat into electricity. This study aims to valorize natural resources, and potentially reduce production costs, by incorporating tetrahedrite-tennantite (td) ores from the Portuguese Iberian Pyrite Belt into synthetic samples. The ore samples were collected in a mine waste at Barrig & atilde;o and as "dirty-copper" pockets of ore from the Neves Corvo mine. Subsequently, high-energy ball milling and hot pressing were employed in the production of thermoelectric materials. These are characterized by XRD, SEM/EDS, and thermoelectrical properties. The complete dissolution of the dump material sulfides with the synthetic tetrahedrite constituents led to an increase in the amount of the tetrahedrite-tennantite phase, which was made up of a tetrahedrite-tennantite-(Fe) solid solution. The thermoelectric characterization of these materials is provided, revealing that most of the combined synthetic ore samples displayed better results than the pristine tetrahedrite, mostly due to higher Seebeck coefficient values. Furthermore, the best thermoelectric performance is achieved with 10% of ore, where a power factor of 268 mu W.K-2.m-1 is reached at room temperature.
  • Exploring Marine Biomineralization on the Al-Mg Alloy as a Natural Process for In Situ LDH Growth to Improve Corrosion Resistance
    Publication . Marques, Maria João; Mercier, Dimitri; Seyeux, Antoine; Zanna, Sandrine; Tenailleau, Christophe; Duployer, Benjamin; Jeannin, Marc; Marcus, Philippe; Basséguy; BASSEGUY, Regine
    ABSTRACT: This study provides a detailed characterization of the AA5083 aluminum alloy, surface, and interface over 6 months of immersion in seawater, employing techniques such as SEM/EDX, GIXRD, mu-Raman and XPS. The purpose was to evaluate the evolution of the biomineralization process that occurs on the Al-Mg alloy. By investigating the specific conditions that favor the in situ growth of layered double hydroxide (LDH) during seawater immersion as a result of biomineralization, this research provides insights into marine biomineralization, highlighting its potential as an innovative and sustainable strategy for corrosion protection.
  • Evolution of atomically dispersed co-catalysts during solar or UV photocatalysis for efficient and sustained H2 production
    Publication . Capelo, Anabela; Fattoruso, Domenico; Valencia-Valero, Laura; Esteves, M. Alexandra; Rangel, Carmen M.; Puga, Alberto
    ABSTRACT: The evolution of metal/titania photocatalysts during photocatalytic H-2 evolution is herein studied. Samples containing atomically dispersed Pt co-catalysts (single atoms, clusters and sub-nanoparticles) formed after calcination were compared to pre-reduced analogues mostly having metallic nanoparticles (diameters >1 nm) during ethanol photoreforming under either UV-rich irradiation or natural sunlight. Aggregation of ultra-dispersed oxidised platinum entities (Pt delta+) with concomitant reduction into Pt-0 nanoparticles (1-2 nm) was observed after UV irradiation by transmission electron microscopy (TEM), and diffuse reflectance UV-visible (DRUV-vis) and X-ray photoelectron (XPS) spectroscopies. A parallel, albeit slower, evolution trend was evidenced during solar photocatalysis. Conversely, atomically dispersed Cu co-catalyst species did not grow and became in-situ reduced into sub-nanometric Cu-0 under irradiation. Hydrogen production rates were remarkably high during initial stages of UV irradiation, and then declined to a sustained regime (approximate to 50 and 8 mmol g(-1) h(-1) for Pt/TiO2 or Cu/TiO2, respectively, for up to 24 h of irradiation). Steadier solar photoreforming was observed in experiments performed in a compound parabolic collector tubular reactor (approximate to 7.6 and 1.7 mmol g(-1) h(-1) for Pt/TiO2 or Cu/TiO2, respectively). Despite the non-negligible effect of co-catalyst rearrangement on activity rationalised herein, attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy measurements pre- and post-photocatalysis suggest that accumulation of strongly adsorbed degradation intermediates, chiefly acetate, is a major cause for rate decreases. Notwithstanding, this phenomenon did not result in total deactivation, so that sustained hydrogen production upon long-term irradiation was not compromised.
  • Detection of corrosion on silvered glass reflectors via image processing
    Publication . Wiesinger, Florian; Baghouil, Sarah; Le Baron, Estelle; Collignon, Romain; Santos, Filipa; Cunha Diamantino, Teresa; Catarino, Isabel; Facão, Jorge; Ferreira, Cristina; Páscoa, Soraia; Sutter, Florian; Fernández-García, Aránzazu; Wette, Johannes
    ABSTRACT: A novel characterization technique based on image analysis is presented, intended to complement state-of-the-art reflectometer measurements. The technique is developed by experts from different laboratories (OPAC, AGC, CEA and LNEG), which subsequently conduct two Round Robin experiments on corroded solar reflectors for validation. Regarding the inter-comparability, it is found that parameters like the corrosion spot density or the penetration maximum on coated edges exhibit an average coefficient of variation of 62.6 % and 54.9 %. Better agreement is found for parameters like the total corroded area and the maximum edge corrosion penetration, with coefficients of variation of 14.3 % and 13.4 %, respectively. The developed methodology is further applied during a 68-month lasting outdoor exposure campaign of two types of solar reflectors at two representative sites, one exhibiting corrosivity class C2 and the other C3. On the commercial coating RL1, a total corroded area of 59 mm2 and 426 mm2 is measured after the outdoor exposure on the C2 and the C3 site, respectively, while on the novel low-lead coated reflector RL3 corresponding values are 280 mm2 and 1308 mm2. This shows the superior quality of the coating RL1 in terms of corrosion resistance. Furthermore, the analysis highlights the importance of proper edge sealing for corrosion protection, since corrosion penetration is increased by a factor between 1.3 and 4.0 if the edges are unprotected. The reflectance decrease after the outdoor exposure is regarded as negligible (0.000 - 0.005), thus not permitting any of the conclusions that are made from the novel image analysis technique.
  • Simulation of Surface Segregation in Nanoparticles of Pt-Pd Alloys
    Publication . Correia, Jose B.; Sá, Ana
    ABSTRACT: Platinum (Pt) and palladium (Pd) are crucial in hydrogen energy technologies, especially in fuel cells, due to their high catalytic activity and chemical stability. Pt-Pd nanoparticles, produced through various methods, enhance catalytic performance based on their size, shape, and composition. These nanocatalysts excel in direct methanol fuel cells (DMFCs) and direct ethanol fuel cells (DEFCs) by promoting alcohol oxidation and reducing CO poisoning. Pt-Pd catalysts are also being explored for their oxygen reduction reaction (ORR) on the cathodic side of fuel cells, showing higher activity and stability than pure platinum. Molecular dynamics (MD) simulations have been conducted to understand the structural and surface energy effects of PdPt nanoparticles, revealing phase separation and chemical ordering, which are critical for optimizing these catalysts. Pd migration to the surface layer in Pt-Pd alloys minimizes the overall potential energy through the formation of Pd surface monolayers and Pt-Pd bonds, leading to a lower surface energy for intermediate compositions compared to that of the pure elements. The potential energy, calculated from MD simulations, increases with a decreasing particle size due to surface creation, indicating higher reactivity for smaller particles. A general contraction of the average distance to the nearest neighbour atoms was determined for the top surface layers within the nanoparticles. This research highlights the significant impact of Pd segregation on the structural and surface energy properties of Pt-Pd nanoparticles. The formation of Pd monolayers and the resulting core-shell structures influence the catalytic activity and stability of these nanoparticles, with smaller particles exhibiting higher surface energy and reactivity. These findings provide insights into the design and optimization of Pt-Pd nanocatalysts for various applications.
  • Investigation of the Effect of Milling Time on Elemental Powders of Oxi-Reduction Nickel and Hydrogenation : Dehydrogenation Titanium
    Publication . Teixeira, Rodolfo da Silva; Gurgel, Mônica Aline Magalhães; Rodrigues, Patricia Freitas; Freitas, Bruno Xavier de; Le Sénéchal, Naiara; Oliveira, R. V.; Neves, Filipe; Paula, Andersan dos Santos
    ABSTRACT: Mechanical alloying (MA) is widely applied in the synthesis of blended elemental or prealloyed powders. This work evaluates the effect of milling time on elemental nickel and titanium powders produced by oxi-reduction and the hydrogenation-dehydrogenation process, respectively. The powders are characterized by scanning electron microscopy, X-ray diffraction, particle size, powder yield, and differential scanning calorimetry. It is observed that increasing the milling time promotes the formation of a structure composed of thin lamellae of nickel and titanium, which results in the beneficial effect of lowering the temperature for the formation of the intermetallic of the Ni-Ti system and in the powder yield achieved. The reduction of milling time in the MA process of NiTi alloys enhances technological efficiency by decreasing their overall processing time.
  • The START project: Transforming mining waste into waste heat recovery materials
    Publication . Neves, Filipe; Vicenzi, Bruno
    ABSTRACT: The START project aims to produce thermoelectric devices for waste heat recovery applications from secondary mineral resources (mining waste).
  • Thermal Shock Resistance of Commercial Oxide-Bonded Silicon Carbide Reticulated Foams under Concentrated Solar Radiation at PSA: A Feasibility Study
    Publication . Oliveira, Fernando Almeida Costa; Galindo, José; Rodriguez, Jose; Cañadas, Inmaculada; Fernandes, Jorge Cruz
    ABSTRACT: Volumetric ceramic receivers can be regarded as a promising technology to heat air above 1000 ◦C for solar thermal electricity production. In this study, the thermal shock behavior of commercial 10 ppi (A) and 20 ppi (B) oxide-bonded silicon carbide (ob-SiC) reticulated porous ceramic (RPC) foams was evaluated using the SF60 solar furnace at Plataforma Solar de Almería. The foams were subjected to well-controlled temperature cycles ranging from 800 to 1000, 1200, 1300 or 1400 ◦C, for 25, 100, and 150 cycles. The extent of the damage after thermal shock was determined by crushing tests. The damage was found to be critically dependent on both the bulk density and cell size. Decreasing both the bulk density and cell size resulted in better thermal shock resistance. The B foam exhibited approximately half the stress degradation compared to the A foam when exposed to a temperature difference of 600 K (in the range of 800 to 1400 ◦C) and subjected to 150 cycles.
  • New triazinephosphonate dopants for Nafion proton exchange membranes (PEM)
    Publication . Teixeira, Fatima; Teixeira, António P. S.; Rangel, C. M.
    ABSTRACT: A new paradigm for energy is underway demanding decarbonized energy systems. Some of them rely on emerging electrochemical devices, crucial in hydrogen technologies, including fuel cells, CO 2 and water electrolysers, whose applications and performances depend on key components such as their separators/ion-exchange membranes. The most studied and already commercialized Nafion membrane shows great chemical stability, but its water content limits its high proton conduction to a limited range of operating temperatures. Here, we report the synthesis of a new series of triazinephosphonate derivatives and their use as dopants in the preparation of new modified Nafion membranes. The triazinephosphonate derivatives were prepared by substitution of chlorine atoms in cyanuric chloride. Diverse conditions were used to obtain the trisubstituted (4-hydroxyphenyl)triazinephosphonate derivatives and the (4-aminophenyl)triazinephosphonate derivatives, but with these amino counterparts, only the disubstituted compounds were obtained. The new modified Nafion membranes were prepared by casting incorporation of the synthesized 1,3,5-triazinephosphonate (TPs) derivatives. The evaluation of the proton conduction properties of the new membranes and relative humidity (RH) conditions and at 60 degrees C, showed that they present higher proton conductivities than the prepared Nafion membrane and similar or better proton conductivities than commercial Nafion N115, in the same experimental conditions. The Nafion-doped membrane with compound TP2 with a 1.0 wt % loading showed the highest proton conductivity with 84 mScm - 1 .