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The fabrication of low-electrical-percolation-threshold polymer composites aims to reduce the weight fraction of the conductive nanomaterial necessary to achieve a given level of electrical resistivity of the composite. The present work aimed at preparing composites based on multiwalled carbon nanotubes (MWCNTs) and magnetite particles in a polyurethane (PU) matrix to study the effect on the electrical resistance of electrodes produced under magnetic fields. Composites with 1 wt.% of MWCNT, 1 wt.% of magnetite and combinations of both were prepared and analysed. The hybrid composites combined MWCNTs and magnetite at the weight ratios of 1:1; 1:1/6; 1:1/12; and 1:1/24. The results showed that MWCNTs were responsible for the electrical conductivity of the composites since the composites with 1 wt.% magnetite were non-conductive. Combining magnetite particles with MWCNTs reduces the electrical resistance of the composite. SQUID analysis showed that MWCNTs simultaneously exhibit ferromagnetism and diamagnetism, ferromagnetism being dominant at lower magnetic fields and diamagnetism being dominant at higher fields. Conversely, magnetite particles present a ferromagnetic response much stronger than MWCNTs. Finally, optical microscopy (OM) and X-ray micro computed tomography (micro CT) identified the interaction between particles and their location inside the composite. In conclusion, the combination of magnetite and MWCNTs in a polymer composite allows for the control of the location of these particles using an external magnetic field, decreasing the electrical resistance of the electrodes produced. By adding 1 wt.% of magnetite to 1 wt.% of MWCNT (1:1), the electric resistance of the composites decreased from 9 × 104 to 5 × 103 Ω. This approach significantly improved the reproducibility of the electrode’s fabrication process, enabling the development of a triboelectric sensor using a polyurethane (PU) composite and silicone rubber (SR). Finally, the method’s bearing was demonstrated by developing an automated robotic soft grip with tendon-driven actuation controlled by the triboelectric sensor. The results indicate that magnetic patterning is a versatile and low-cost approach to manufacturing sensors for soft robotics.

The use of vegetable oils to produce biodiesel raises several sustainability issues, namely the fuel/food conflict. The high cost of vegetable oils and an expensive homogeneous base catalyzed process encourages the search for alternative raw materials and more efficient production processes. Biodiesel from beef tallow, a non-edible fat, was produced by methanolysis over calcium based heterogeneous catalyst. The catalyst was prepared by calcination of scallop shells at 800 ​°C. To overcome the undesired effect of the tallow acidity (3.9 mgKOH/gfat), mixtures of tallow and soybean oil (SBO) (0.6 mgKOH/gfat) were processed and alcohol co-solvents (isopropanol, 1-propanol, and isobutanol) and biodiesel itself, as a solvent, were used to improve the miscibility of the reaction mixture. Processing of neat tallow promotes an important decay of the catalytic activity due to the partial neutralization of the basic catalyst. Co-processing mixtures of tallow/SBO allowed minimizing the acidity effect. Alcohol co-solvents harmed the biodiesel yield due to competitive adsorption of alcohols with methanol on catalyst active sites but protected the catalyst against adsorption of the reaction mixture species. Biodiesel used as a solvent had an almost null effect on the esterification reaction yield, thus showing the absence of mass transfer limitation. Co-processing low-grade fat with vegetable oil seems to be a feasible strategy to process low-grade fats using basic heterogeneous catalysts, thus contributing to improving the sustainability of biodiesel production.

The on-board identification of ore minerals during a cruise is often postponed until long after the cruise is over. During the M127 cruise, 21 cores with deep-seafloor sediments were recovered in the Trans-Atlantic Geotraverse (TAG) field along the Mid Atlantic Ridge (MAR). Sediments were analyzed on-board for physicochemical properties such as lightness (L*), pH and Eh. Selected samples were studied for mineral composition by X-ray powder diffraction (XRD). Based on XRD data, sediment samples were separated into high-, low- and non-carbonated. Removal of carbonates is a common technique in mineralogical studies in which HCl is used as the extraction agent. In the present study, sequential extraction was performed with sodium acetate buffer (pH 5.0) to remove carbonates. The ratio between the highest calcite XRD reflection in the original samples (Iorig) vs its XRD-reflection in samples after their treatment with the buffer (Itreat) was used as a quantitative parameter of calcite removal, as well as to identify minor minerals in carbonated samples (when Iorig/Itreat &gt, 24). It was found that the lightness parameter (L*) showed a positive correlation with calcite XRD reflection in selected TAG samples, and this could be applied to the preliminary on-board determination of extraction steps with acetate buffer (pH 5.0) in carbonated sediment samples. The most abundant minerals detected in carbonated samples were quartz and Al- and Fe-rich clays. Other silicates were also detected (e.g., calcic plagioclase, montmorillonite, nontronite). In non-carbonated samples, Fe oxides and hydroxides (goethite and hematite, respectively) were detected. Pyrite was the dominant hydrothermal mineral and Cu sulfides (chalcopyrite, covellite) and hydrothermal Mn oxides (birnessite and todorokite) were mineral phases identified in few samples, whereas paratacamite was detected in the top 20 cm of the core. The present study demonstrates that portable XRD analysis makes it possible to characterize mineralogy at cored sites, in particular in both low- and high-carbonated samples, before the end of most cruises, thus enabling the quick modification of exploration strategies in light of new information as it becomes available in near-real time.

Calcium diglyceroxide (CaD) was used as the catalyst for biodiesel production through oil methanolysis. It was evaluated its catalytic behavior, its air expo- sure tolerance, and the Ca leaching. CaD catalyst was synthesized from food waste scallop shell derived CaO (obtained by calcination at 900 °C) by contacting with a mixture of equal volumes of glycerin and methanol at 65 °C for 2 h. The CaO obtained by calcination of scallop shell was used as reference catalyst. In standard reaction conditions (2.5 h, methanol reflux temperature, 5 wt% (oil basis) catalyst loading, and methanol:oil = 12:1 moral ratio), CaD presented lower catalytic activity than CaO (FAME yield of 92% against 99%, respectively). 24 h repined CaD presented improved catalytic behavior probably due to the formation of surface Ca −OH groups, achieving 96% of FAME yield. Thermogravimetry (TG) data showed that inorganic residue was larger for biodiesel than for glycerin, being CaD catalyst more soluble than CaO. Data showed that CaD is unstable under reaction conditions, suffering leaching, but the absence of Matter Organic Non-Glycerol (MONG) in the glycerin phase allows to neglect the homogeneous contribution of the leached catalyst. CaD formation during reaction contributes to FAME contamination with Ca and promotes catalyst deactivation thus being an undesired occurrence.

11 páginas.-- 6 figuras.-- 1 tablas- 67 referencias.-- Supplementary information accompanies this paper at https://doi.org/10.1038/s41598-018-20393-2, Microbial diversity in lava tubes from Canary Islands (Spain) has never been explored thus far offering a unique opportunity to study subsurface microbiology. Abundant yellow coloured mats developing on coralloid speleothems in a lava tube from La Palma Islands were studied by next-generation sequencing and DNA/RNA clone library analyses for investigating both total and metabolically active bacteria. In addition, morphological and mineralogical characterization was performed by field emission scanning electron microscopy (FESEM), micro-computed tomography, X-ray diffraction and infrared spectroscopy to contextualize sequence data. This approach showed that the coralloid speleothems consist of banded siliceous stalactites composed of opal-A and hydrated halloysite. Analytical pyrolysis was also conducted to infer the possible origin of cave wall pigmentation, revealing that lignin degradation compounds can contribute to speleothem colour. Our RNA-based study showed for the first time that members of the phylum Actinobacteria, with 55% of the clones belonging to Euzebyales order, were metabolically active components of yellow mats. In contrast, the DNA clone library revealed that around 45% of clones were affiliated to Proteobacteria. Composition of microbial phyla obtained by NGS reinforced the DNA clone library data at the phylum level, in which Proteobacteria was the most abundant phylum followed by Actinobacteria., Tis research was supported by the Spanish Ministry of Economy, Industry and Competitiveness (MINEICO), project CGL2013–41674-P. J.L.G-P. and A.Z.M. were supported by a PhD fellowship (BES-2014–069587) and a “Juan de la Cierva – Incorporación” post-doctoral contract (IJCI-2014–20443) from the MINEICO, respectively. Te Portuguese Foundation for Science and Technology (Strategic project UID/ECI/04028/2013) are also thanked for fnancial support. Te authors would like to thank the assistance during the feld work and photographic contributions in La Palma lava tubes of the speleologist Octavio Fernandez. We gratefully acknowledge the collecting permissions granted by the staf of Caldera del Taburiente National Park (La Palma Island, Spain).

Lithium extraction from hard-rock ores has regained importance due to the increased demand for this metal to supply the growing battery market. Therefore, several studies have been focused on the lithium extraction from ores, however, leaching and purification steps are sparsely studied. Thus, the objective of this study was to evaluate the main factors affecting the water leaching step and the subsequent purification operations for lithium recovery from a lepidolite concentrate, which was processed by mechanical activation and sulphuric acid digestion. In the leaching step, among the variables studied, only one, the leaching temperature, showed a significant effect on the lithium extraction, taking into account the range of values tested. Thus, the recommended operating value for the leaching time and the L/S ratio is the minimum, while for the leaching temperature is 50°C. After optimizing the leaching operation, the purification of the leachate, by neutralization, was thoroughly performed by efficient removal of impurities (Fe, Al, Mn and Ca), allowing to obtain lithium carbonate as final product, as well as other relevant by-products, such as rubidium and potassium alums. info:eu-repo/semantics/publishedVersion

The hydrometallurgical extraction of metals from spent lithium-ion batteries (LIBs) was investigated. LIBs were first dismantled and a fraction rich in the active material was obtained by physical separation, containing 95% of the initial electrode, 2% of the initial steel and 22% of plastic materials. Several reducers were tested to improve metals dissolution in the leaching step using sulphuric acid. Sodium metabisulphite led to the best results and was studied in more detail. The best concentration of Na2S2O5 was 0.1 M. The metals dissolution increased with acid concentration, however, concentrations higher than 1.25 M are unnecessary. Best results were reached using a stirring speed of 400 min(-1). The metals leaching efficiency from the active material (Li, Mn, Ni, Co) increased with the temperature and was above 80% for temperatures higher than 60 degrees C. The dissolution of metals also rose with the increase in the liquid/solid ratio (LAS), however, extractions above 85% can be reached at LAS as lower as 4.5 L/kg, which is favourable for further purification and recovery operations. About 90% of metals extraction can be achieved after only 0.5 h of leaching. Sodium metabisulphite can be an alternative reducer to increase the leaching of Li, Mn, Co, and Ni from spent LIBs. info:eu-repo/semantics/publishedVersion

An excavation in a 14th c. church at Torres Novas, named Santa Maria do Castelo, provided some green glazed ceramic sherds, archaeologically dated from 14th c. to the 16th c. The town of Torres Novas is located at the center of Portugal, about 100 km north of Lisbon. The obtained results evidence three types of pastes of the pottery: type 1 with Quartz, Illite, Muscovite and Microcline as the main constituents, type 2 with Quartz, Calcite and Gehlenite; and finally type 3 with Quartz, Calcite and Diopside being the major components. Type 1 pastes are related to clay sources of Pliocene origin, and all this pottery was most probably made in Portuguese kilns. However, types 2 and 3 spectroscopic trends are remarkably different, indicating that those ceramics were produced in Seville. All the studied ceramics are lead glazed, and green glazed. In one of the samples from the Seville kiln, Cerusite was the main pigment used to obtain the greenish colouration. In what regards the origin of all samples produced with Pliocene clays, the 16th c. ones were most likely produced in the Santo Antonio da Charneca or Mata da Machada kilns, both located in the south shore of the Tagus river, region of Lisbon. In what regards the green glazed jug rim (14th c.) and the jug spout (15th c.) they could also have been produced in the two mentioned kilns south of Lisbon city, but another interesting hypothesis - due to richness of the decoration - is the production in Lisbon workshops, with the use of Pliocene clays imported by Lisbon potters, now documented both in Lisbon archaeological findings and also in documental sources.

This paper assesses the physical, chemical and mineralogical characteristics of fine recycled aggregates obtained from crushed concrete waste, comparing them with two types of natural fine aggregates from different origins. A commercial concrete was jaw crushed, and the effect of different aperture sizes on the particle size distribution of the resulting aggregates was evaluated. The density and water absorption of the recycled aggregates was determined and a model for predicting water absorption over time is proposed. Both natural and recycled aggregates were characterized regarding bulk density and fines content. Recycled aggregates were additionally characterized by XRD, SEM/EDS and DTA/TG of individual size fractions. The results show that natural and recycled fine aggregates have very different characteristics. This should be considered in potential applications, both in terms of the limits for replacing amounts and of the rules and design criteria of the manufactured products.

Cellulose acetate (CA)–silver (Ag) nanocomposite asymmetric membranes were prepared via the wet-phase inversion method by dispersing polyvinylpirrolydone-protected Ag nanoparticles in the membrane casting solutions of different compositions. Silver nanoparticles were synthesized ex situ and added to the casting solution as a concentrated aqueous colloidal dispersion. The effects of the dispersion addition on the structure and on the selective permeation properties of the membranes were studied by comparing the nanocomposites with the silver-free materials. The casting solution composition played an important role in the adequate dispersion of the silver nanoparticles in the membrane. Incorporation of nanoscale silver and the final silver content resulted in structural changes leading to an increase in the hydraulic permeability and molecular weight cut-off of the nanocomposite membranes. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41796.

The aim of this study is to apply X-ray microfocus computed microtomography (μ-XCT), a promising non-destructive 3D microscopy imaging technique, based on measurements of X-ray linear path attenuation coefficient, in order to study a Portuguese travertine, a random heterogeneous geomaterial used in urban heritage constructions. This study evaluates the impact of soluble sulphate salt–induced decay phenomena on texture characteristics at a micrometric scale. This is done to better describing, imaging, measuring and understanding the impact of an artificially induced sulphate-decay process on petrographic/petrophysical properties. A Portuguese travertine was chosen as the object of our study. Its laboratory-induced changes were systematically monitored, using non-destructive techniques, to determine voids (pores + fractures)/matrix fractions and size spectrum evolution based on 3-D images. This investigation demonstrates that the μ-XCT potential constitutes a valid complementary tool when analysing decay processes of complex natural materials in different environmental conditions. It clearly provides suggestive and important qualitative and/or quantitative estimates, at different spatial scales, of environmentally induced stone voids/matrix network spatial structure-texture evolution correlations. Further qualitative/quantitative parameterization assessment and statistical validation will be the next step to be taken on this study., Fundação para a Ciência e a Tecnologia (FCT) através do projeto POCTI\CTA\44940\2002_PORENET e os projetos estratégicos PEstOE/CTE/UI0697/2011 and PEst-OE/CTE/UI0098/2011 (fundos nacionais e europeus - FEDER)