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- Comparison of the corrosion of ferritic and austenitic stainless steel (AISI 430 and AISI 316L) with LiNaK carbonate salts for thermal energy storage in CSP/CST applicationsPublication . Gil, Mafalda; Pedrosa, Fátima; Paiva Luís, Teresa; Figueira Vasques, Isabel; Oliveira, Fernando; Cunha Diamantino, TeresaABSTRACT: This study focuses on the corrosion rates and mechanisms of two stainless steels, austenitic AISI 316L and ferritic AISI 430, in contact with a eutectic mixture of LiNaK carbonates in long-term tests at 650 degrees C. The selection of these two stainless steels was based on their differences, both in their intrinsic characteristics and in the cost associated with each one. The research also underscores the importance of optimizing the descaling methods used to evaluate the corrosion rate. Corrosion rates were measured gravimetrically according to ISO 17245:2015, revealing an asymptotic behavior for both steels, with AISI 430 with a corrosion rate of 237 f 21 mu m and AISI 316L of 151 f 13 mu m after 2000 h of testing. Corrosion mechanisms were analyzed using SEM/EDS, GDOES, and XRD techniques, which identified well-defined oxide layers with varying compositions. Given the observed corrosion mechanisms and its lower cost, AISI 430 steel seems to have great applicability in CSP/CST plants, provided it is paired with an appropriate protective coating.
- Detection of corrosion on silvered glass reflectors via image processingPublication . 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, JohannesABSTRACT: 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.
- Determination of reflectance of interest from limited state-of-the-art solar reflector field soiling measurementsPublication . Wette, Johannes; Sutter, Florian; Cunha Diamantino, Teresa; Montecchi, Marco; Bern, Gregor; Fernández-García, AránzazuABSTRACT: In concentrated solar thermal technologies, plant operators usually monitor the soiling of their solar field with handheld reflectometers. These measurements can be used for yield calculations and to adapt cleaning strategies: if the reflectometer reading falls below an empirically established threshold, the solar field should be cleaned. There are several commercial reflectometers available for this purpose, but all of them measure at different combinations of wavelength, acceptance angle or incidence angle. It is the purpose of this study to bring the readings from all main commercial reflectometers to the same representative value, enabling their comparison with one another and the translation of these readings into a meaningful reflectance parameter. Thus, different handheld reflectometers are correlated with a laboratory reflectometer, capable of measuring in the whole solar spectral region, covering a wide range of incidence and acceptance angles. The most significant parameter is the near-specular solar-weighted reflectance, measured at the typical incidence and acceptance angles for a given plant, as it is the most precise parameter to describe the reflected energy from the solar field. The correlations for all included reflectometers, show highly linear correlations over a wide range of soiling levels with low deviations. Consequently, the correlations presented herein enable the plant operators at the studied site to compute the near-specular solar-weighted reflectance from their reflectometer readings. and, with that, increase the significance of the measurements without collecting any additional data. The work also establishes a detailed procedure to derive this type of correlations at any site of interest.
- Enhanced borohydride oxidation kinetics with Au@MOF-808 nanocomposite electrocatalysts with ultra-low Au loadingPublication . Belhaj, Ines; Becker, J. Alexander; Viana, Alexandre M.; Gusmão, Filipe M. B.; Chaves, Miguel; Pereira, Eulália; Sljukic, Biljana; Balula, Salete S.; Silva, Luis Cunha; Santos, Diogo M. F.ABSTRACT: The highly stable metal-organic framework (MOF) composed of[Zr6O4(mu 3-OH)4(OH)6(H2O)6(BTC)2]& sdot;nH2O units (MOF-808) was modified by incorporating gold (Au) nanoparticles and functional groups to enhance electrocatalytic activity for the borohydride oxidation reaction (BOR). Three composite materials (Au@MOF-808, Au@MOF-808-NH2, and Au@MOF-808-SH) were prepared by the incorporation of Au in structurally related MOFs, MOF-808, MOF-808-NH2, and MOF-808-SH, respectively. These composite materials were evaluated as anodic electrocatalysts for BOR in alkaline media using cyclic voltammetry and chronoamperometry. Among the prepared materials, Au@MOF-808-NH2 exhibited the highest BOR activity, with an apparent activation energy of 15.3 kJ mol-1, a reaction order of 0.6, an anodic charge transfer coefficient of 0.63, and a number of exchanged electrons of 4.4. The latter was significantly below the theoretical eight-electron value, indicating the presence of alternative reaction pathways. Notably, this material achieved a high mass-specific BOR peak current of 4.23 A mu gAu-1, demonstrating outstanding electrocatalytic efficiency despite the ultralow noble metal loading. These results underscore the potential of Au@MOF-808-NH2 as a cost-effective and scalable anodic electrocatalyst for high-performance direct borohydride fuel cells.
- Exploring Marine Biomineralization on the Al-Mg Alloy as a Natural Process for In Situ LDH Growth to Improve Corrosion ResistancePublication . Marques, Maria João; Mercier, Dimitri; Seyeux, Antoine; Zanna, Sandrine; Tenailleau, Christophe; Duployer, Benjamin; Jeannin, Marc; Marcus, Philippe; Basséguy; BASSEGUY, RegineABSTRACT: 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.
- Influence of Cr on the quaternary FeTaTiW medium entropy alloyPublication . Martins, Ricardo; Monteiro, Bernardo; Pereira Gonçalves, Antonio; Correia, Jose B.; Galatanu, Andrei; Alves, Eduardo; Tejado, Elena; Pastor, Jose Ygnacio; Dias, MartaABSTRACT: The search for advanced materials has been growing, and high entropy alloys (HEAs) are emerging as promising candidates for application in the fusion domain. This work investigates the effect of Cr on the FeTaTiW medium entropy alloy to form (CrFeTaTi)70W30 high entropy alloy, comparing the experimental production and characterization with the simulation (molecular dynamics and hybrid molecular dynamics-Monte Carlo) of the phases formed. The alloys were produced by mechanical alloying and sintered by spark plasma sintering. Both simulations have shown that a body-centered cubic structure is formed for both compositions. Monte Carlo simulation provides a more precise prediction of microstructural formation and element segregation. Microstructural examination of the consolidated material revealed the presence of a W-rich phase and a Ti-rich phase, consistent with the phase separation observed in the MC simulations. Moreover, X-ray diffraction analysis of the milled powder for FeTaTiW and (CrFeTaTi)70W30 confirmed the formation of a bcc (body-centered cubic)-type structure with a low fraction of intermetallic phases. Mechanical testing showed ductile behavior at 1000 degrees C where (CrFeTaTi)70W30 showed a stress magnitude almost double that of FeTaTiW. Additionally, the thermal diffusivity between 20 and 1000 degrees C of both alloys increases as the temperature rises. (CrFeTaTi)70W30 exhibits an increase from 3 to 5 mm2/s, while FeTaTiW increases from 4 to 9 mm2/s. Still, both system's thermal diffusivity values are lower than those of CuCrZr and pure tungsten. Despite this, the study underscores the promising attributes of HEAs and highlights areas for further optimization to enhance its suitability for extreme conditions.
- Mechanical Performance of Ceria-Coated 3D-Printed Black Zirconia Cellular Structures After Solar Thermochemical CO/H2 Fuel Production CyclesPublication . Oliveira, Fernando; Sardinha, Manuel; Justino Netto, Joaquim Manoel; Leite, Marco; Farinha, Miguel; Barreiros, Maria Alexandra; Abanades, Stéphane; Fernandes, JorgeABSTRACT: Solar fuels production requires developing redox active materials with porous structures able to withstand thermochemical cycles with enhanced thermal stability under concentrated solar irradiation conditions. The mechanical performance of 3D-printed, macroporous black zirconia gyroid structures, coated with redox-active ceria, was assessed for their suitability in solar thermochemical cycles for CO2 and H2O splitting. Experiments were conducted using a 1.5 kW solar furnace to supply the high-temperature concentrated heat to a windowed reaction chamber to carry out thermal redox cycling under realistic on-sun conditions. The ceria coating on ceramic structures improved the thermal stability and redox efficiency while minimizing the quantity of the redox material involved. Crushing strength measurements showed that samples not directly exposed to the concentrated solar flux retained their mechanical performance after thermal cycling (similar to 10 MPa), while those near the concentrated solar beam focus exhibited significant degradation due to thermal stresses and the formation of CexZr1-xO2 solid solutions (similar to 1.5 MPa). A Weibull modulus of 8.5 was estimated, marking the first report of such a parameter for fused filament fabrication (FFF)-manufactured black zirconia with gyroid architecture. Failure occurred via a damage accumulation mechanism at both micro- and macro-scales. These findings support the viability of ceria-coated cellular ceramics for scalable solar fuel production and highlight the need for optimized reactor designs.
- New Modified SPEEK-Based Proton Exchange MembranesPublication . Teixeira, Fatima; Teixeira, António Paulo Silva; Rangel, Carmen M.ABSTRACT: A decarbonized society demands cleaner and sustainable energy sources based on well-established or emerging technologies with the potential to make a significant contribution to energy storage and conversion, such as batteries, fuel cells and water and/or CO2 electrolyzers. The performance of these electrochemical devices relies on key components such as their separators/ion-exchange membranes. The most common commercial membrane, Nafion (R), has several technological limitations. In this study, it is proposed the incorporation of bisphosphonic acid (BP) dopants into membrane matrices to improve their properties. Following this strategy, we prepared new membranes based on sulfonated poly(etheretherketone) (SPEEK) polymer, a reliable and effective alternative membrane polymer, through the incorporation of the BP dopants, to obtain low-cost membranes with improved properties. These membranes were structural, thermal and morphological, characterized by AT-FTIR, TGA and SEM. Their proton conductivity was evaluated over a temperature range between 30 degrees C and 60 degrees C, using Electrochemical Impedance Spectroscopy, and their stability during this process was also observed. The best proton conductivity was observed for the SPEEK membrane doped with BP1 at 2.0 wt% load at 60 degrees C, with a proton conduction of 226 mS cm-1.
- New proton exchange membranes based on ionic liquid doped chitosanPublication . Naffati, Naima; Teixeira, Fatima; Teixeira, António Paulo Silva; Rangel, Carmen M.ABSTRACT: The development of new proton exchange membranes (PEM) for electrochemical devices have attracted researcher's attention in the pursuit for more sustainable and cost-effective technologies for clean energy production and conversion. In this work, new doped chitosan (CS) membranes were prepared by the casting method. Chitosan is an abundant, biodegradable and non-toxic material, and as a membrane, a sustainable and cheaper alternative to those perfluorinated and commonly used, such as Nafion. Three different ionic liquids were employed as dopants, ([EMIM][OTf], [EMIM][FSI] and [MIMH][HSO4]), in various concentrations and up to 50 wt% load. The new membranes were characterized by ATR-FTIR, thermogravimetry, using TGA and DSC techniques to assess their thermal properties, and by SEM, to analyse their surface morphology. Proton conduction properties of the new membranes were assessed by Electrochemical Impedance Spectroscopy (EIS). The new doped membranes showed an increase in the proton conduction compared with pristine chitosan membranes. The incorporation of ionic liquids into chitosan membranes improved their proton conductivity and thermal properties, with [EMIM][OTf] and [MIMH][HSO4] showing the most promising results. A 2-fold increment in the proton conduction was generally observed with the increase of the temperature from 30 to 60 degrees C. The best proton conductivity was found at 60 degrees C for the membrane doped with [EMIM][OTf], with a value of 47 mS.cm(-1).
- Novel fast synthesis route for α-MgAgSb thermoelectric materialsPublication . Santos, Beatriz; Sá, Ana; Luz, Paulo P. da; Neves, Filipe; de Boor, Johannes; Pereira Gonçalves, AntonioABSTRACT: Thermoelectric (TE) materials capable of waste heat recovery in the temperature range of 300-525 K remain relatively underdeveloped compared to conventional Bi2Te3-based systems, which present inherent environmental, health, and cost challenges. Recently, MgAgSb-based compounds have garnered significant research interest for applications in this temperature range owing to their intrinsically low thermal conductivity, high figure of merit and higher abundance. However, synthesis of the desired low-temperature alpha-MgAgSb phase typically requires highly controlled production processes-such as multi-step mechanical alloying, followed by extensive, week-long annealing-to mitigate the formation of or transition to undesirable phases. This study proposes an original, rapid, and scalable synthesis strategy combining induction melting for only six minutes with the subsequent classic hot-pressing method. We investigated the effect of nominal stoichiometry on thermoelectric performance by synthesising three distinct compositions: MgAg0.97Sb0.995, MgAg0.965Sb0.985, and MgAg0.955Sb0.985. The MgAg0.955Sb0.985 composition exhibited optimal performance, achieving an average power factor (PF) of 12.8 mu W K-2 cm-1 in the 300-525 K range. By considerably reducing the thermal budget and processing time, this approach significantly improves the energy payback time (EPBT) and reduces the carbon footprint of production, addressing the critical sustainability-performance trade-off that limits large-scale deployment. This result validates the capacity of the proposed fast synthesis route to yield performant MgAgSb-based samples and suggests that the optimal nominal composition is dependent on the specific production technique employed. Fundamentally, this work demonstrates the rapid and successful preparation of the desired alpha-MgAgSb phase using an easily scalable technique that does not require a perpetually inert atmosphere. This process utilises bulky precursor elements directly, significantly reducing production complexity, associated costs, and health hazards. This advancement provides a simpler and more industrially viable pathway for the transition of MgAgSb materials toward commercial availability.