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Influence of Successive Chemical and Thermochemical Treatments on Surface Features of Ti6Al4V Samples Manufactured by SLM

Gonzalez, JE; de Armas, G; Negrin, J; Beltran, AM; Trueba, P; Gotor, FJ; Peon, E; Torres, Y
Metals, 11 (2021) 313
Reactividad de Sólidos


Ti6Al4V samples, obtained by selective laser melting (SLM), were subjected to successive treatments: acid etching, chemical oxidation in hydrogen peroxide solution and thermochemical processing. The effect of temperature and time of acid etching on the surface roughness, morphology, topography and chemical and phase composition after the thermochemical treatment was studied. The surfaces were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction and contact profilometry. The temperature used in the acid etching had a greater influence on the surface features of the samples than the time. Acid etching provided the original SLM surface with a new topography prior to oxidation and thermochemical treatments. A nanostructure was observed on the surfaces after the full process, both on their protrusions and pores previously formed during the acid etching. After the thermochemical treatment, the samples etched at 40 °C showed macrostructures with additional submicro and nanoscale topographies. When a temperature of 80 °C was used, the presence of micropores and a thicker anatase layer, detectable by X-ray diffraction, were also observed. These surfaces are expected to generate greater levels of bioactivity and high biomechanics fixation of implants as well as better resistance to fatigue.

Febrero, 2021 | DOI: 10.3390/met11020313

A Novel, Simple and Highly Efficient Route to Obtain PrBaMn2O5+δ Double Perovskite: Mechanochemical Synthesis

Garcia-Garcia, FJ; Sayagues, MJ; Gotor, FJ
Nanomaterials, 11 (2021) 380
Reactividad de Sólidos


In this work, a mechanochemical route was proposed for the synthesis of the PrBaMn2O5+δ (PMBO) double layered perovskite phase. The mechanochemical reaction between Pr6O11, BaO2, and MnO powders with cationic stoichiometric ratios of 1/1/2 for Pr/Ba/Mn was performed using high-energy milling conditions in air. After 150 min of milling, a new phase with perovskite structure and cubic symmetry consistent with the A-site disordered Pr0.5Ba0.5MnO3 phase was formed. When this new phase was subsequently annealed at a high temperature in an inert Ar atmosphere, the layered PrBaMn2O5+δ phase was obtained without needing to use a reducing atmosphere. At 1100 °C, the fully reduced layered PrBaMn2O5 phase was achieved. A weight gain was observed in the 200–300 °C temperature range when this fully reduced phase was annealed in air, which was consistent with the transformation into the fully oxidized PrBaMn2O6 phase. The microstructural characterization by SEM, TEM, and HRTEM ascertained the formation of the intended PrBaMn2O5+δ phase. Electrical characterization shows very high electrical conductivity of layered PBMO in a reducing atmosphere and suitable in an oxidizing atmosphere, becoming, therefore, excellent candidates as solid oxide fuel cell (SOFC electrodes).

Febrero, 2021 | DOI: 10.3390/nano11020380

Enhanced UV and visible light photocatalytic properties of synthesized AgBr/SnO2 composites

Puga, F.; Navío, J.A.; Hidalgo, M.C.
Separation and Purification Tecnology, 257 (2021) 117948
Fotocatálisis Heterogénea: Aplicaciones


Composites (AgBr/SnO2) comprised of AgBr and SnO2 with different molar % of bare SnO2, have been synthesized by simple precipitation methods; the bare SnO2 used, was synthesized by hydrothermal procedure. Samples have been characterized by X-ray diffraction (XRD), N2-adsorption, UV–vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Photocatalytic activity of the as-prepared photocatalysts was evaluated through photocatalytic degradation of rhodamine B (RhB) and caffeic acid (CAFA) under UV and Visible illumination. In photocatalytic degradation studies, for both substrates, conversion rates of around 95% were found in 45 min of both UV-illumination and 85% under visible lighting. These conversion rates were superior than the conversion rates of pure parental components, AgBr and SnO2 under the same experimental conditions. At least, for RhB no loss of photocatalytic activity has been observed after five recycles although the mineralization degree progressively diminished along the recycles. The enhanced photocatalytic degradation of AgBr/SnO2 compounds was attributed, in part, to a synergistic increase in adsorption viability, as well as to the effective separation of photoinduced load carriers that resulted from the formation of a heterojunction according to the type II junction. Radical scavengers’ experiments indicated that active oxidant species as O2.−, ·OH and h+ all are involved in this photocatalytic system, although it seems that O2.− played the major role in the photocatalytic degrading of RhB by AgBr/SnO2 composites. In summary, coupling AgBr with SnO2 remarkably improves the photocatalytic activity under both UV and visible-illumination with respect to the parental components. These features open the route to future applications of this material in the field of environmental remediation.

Febrero, 2021 | DOI: 10.1016/j.seppur.2020.117948

Guaiacol hydrodeoxygenation in hydrothermal conditions using N-doped reduced graphene oxide (RGO) supported Pt and Ni catalysts: Seeking for economically viable biomass upgrading alternatives

Parrilla-Lahoz, S; Jin, W; Pastor-Perez, L; Carrales-Alvarado, D; Odriozola, JA; Dongil, AB; Reina, TR
Applied Catalysis A-General, 611 (2021) 117977
Química de Superficies y Catálisis


Herein we present an innovative route for model biomass compounds upgrading via “H2-free” hydrodeoxygenation (HDO) reactions. The underlaying idea is to implement a multifunctional catalyst able to activate water and subsequently use in-situ generated hydrogen for the HDO process. In this sense we have developed a series of effective Ni and Pt based catalysts supported on N-promoted graphene decorated with ceria. The catalyst reached commendable conversion levels and selectivity to mono-oxygenated compounds considering the very challenging reaction conditions. Pt outperforms Ni when the samples are tested as-prepared. However, Ni performance is remarkably boosted upon applying a pre-conditioning reductive treatment. Indeed, our NiCeO2/GOr-N present the best activity/selectivity balance and it is deemed as a promising catalyst to conduct the H2-free HDO reaction. Overall, this “proof-concept” showcases an economically appealing route for bio-compounds upgrading evidencing the key role of advanced catalysts for a low carbon future.

Febrero, 2021 | DOI: 10.1016/j.apcata.2020.117977

Photocatalytic oxidation of pollutants in gas-phase via Ag3PO4-based semiconductor photocatalysts: Recent progress, new trends, and future perspectives

Y. Naciri; A. Hsini; A. Bouziani; R. Djellabi; Z. Ajmal; M. Laabd; J.A. Navío; A. Mills; C.L. Bianchi; H.Li; B. Bakiz; A. Albourine
Critical Reviews in Environmental Science and Technology,
Fotocatálisis Heterogénea: Aplicaciones


Air pollution has become a significant challenge for both developing and developed nations. due to its close association with numerous fatal diseases such as cancer, respiratory, heart attack, and brain stroke. Over recent years, heterogeneous semiconductor photocatalysis has emerged as an effective approach to air remediation due to the ease of scale-up, ready application in the field, use of solar light and ready availability of a number of different effective photocatalysts. To date, most work in this area has been conducted using UV-absorbing photocatalysts, such as TiO2 and ZnO; However, recent studies have revealed Ag3PO4 as an attractive, visible-light-absorbing alternative, with a bandgap of 2.43 eV. In particular, this material has been shown to be an excellent photocatalyst for the removal of many types of pollutants in the gas phase. However, the widespread application of Ag3PO4 is restricted due to its tendency to undergo photoanodic corrosion and the poor reducing power of its photogenerated conductance band electrons, which are unable to reduce O2 to superoxide •O2 −. These limitations are critically evaluated in this review. In addition, recent studies on the modification of Ag3PO4 via combination with the conventional heterojunctions or Z-scheme junctions, as well as the photocatalytic mechanistic pathways for enhanced gas-pollutants removal, are summarized and discussed. Finally, an overview is given on the future developments that are required in order to overcome these challenges and so stimulate further research into this promising field.

Febrero, 2021 | DOI: 10.1080/10643389.2021.1877977

Patterning and control of the nanostructure in plasma thin films with acoustic waves: mechanical vs. electrical polarization effects

García-Valenzuela, A.; Fakhouri, A.; Oliva-Ramírez, M.; Rico-Gavira, V.; Rojas, T.C.; Alvarez, R.; Menzel, S.B.; Palmero, A.; Winkler, A.; González-Elipe, A.R.
Materials Horizons, 8 (2021) 515-524
Nanotecnología en Superficies y Plasma - Tribología y Protección de Superficies


Nanostructuration and 2D patterning of thin films are common strategies to fabricate biomimetic surfaces and components for microfluidic, microelectronic or photonic applications. This work presents the fundamentals of a surface nanotechnology procedure for laterally tailoring the nanostructure and crystalline structure of thin films that are plasma deposited onto acoustically excited piezoelectric substrates. Using magnetron sputtering as plasma technique and TiO2 as case example, it is demonstrated that the deposited films depict a sub-millimetre 2D pattern that, characterized by large lateral differences in nanostructure, density (up to 50%), thickness, and physical properties between porous and dense zones, reproduces the wave features distribution of the generated acoustic waves (AW). Simulation modelling of the AW propagation and deposition experiments carried out without plasma and under alternative experimental conditions reveal that patterning is not driven by the collision of ad-species with mechanically excited lattice atoms of the substrate, but emerges from their interaction with plasma sheath ions locally accelerated by the AW-induced electrical polarization field developed at the substrate surface and growing film. The possibilities of the AW activation as a general approach for the tailored control of nanostructure, pattern size, and properties of thin films are demonstrated through the systematic variation of deposition conditions and the adjustment of AW operating parameters.

Febrero, 2021 | DOI: 10.1039/D0MH01540G

Long-term low friction maintenance and wear reduction on the ventral scales in snakes

Sanchez-Lopez, JC; Schaber, CF; Gorb, SN
Materials Letters, 285 (2021) 129011
Tribología y Protección de Superficies


Snake skins evolved to withstand permanent friction and wear during sliding. Here, the microstructure of ventral scales of the snake Lampropeltis getula californiae was analyzed using scanning electron microscopy, and the long-term dynamic friction behavior was investigated by reciprocating sliding friction tests. A smooth epoxy resin with similar elasticity modulus and hardness was used for comparison purposes. Strong differences in frictional and wear mechanisms between the two materials were revealed in spite of similar mechanical properties. Snake skin showed a considerably lower frictional coefficient that kept stable over several thousands of sliding cycles. A reduction of the stick-slip behavior was also denoted by analyzing the variation of the friction coefficient in the forward and reverse motion influencing the wear mechanism. This frictional behavior can be explained by three different but complementary mechanisms: fibrous layered composite material of the skin with a gradient of material properties, surface microstructure, and the presence of ordered layers of lipid molecules at the skin surface.

Febrero, 2021 | DOI: 10.1016/j.matlet.2020.129011

Dysprosium and Holmium Vanadate Nanoprobes as High-Performance Contrast Agents for High-Field Magnetic Resonance and Computed Tomography Imaging

Gomez-Gonzalez, E; Nunez, NO; Caro, C; Garcia-Martin, ML; Fernandez-Afonso, Y; de la Fuente, JM; Balcerzyk, M; Ocana, M
Inorganic Chemistry, 60 (2021) 152-160
Materiales Coloidales


We describe a wet chemical method for the synthesis of uniform and well-dispersed dysprosium vanadate (DyVO4) and holmium vanadate (HoVO4) nanoparticles with an almost spherical shape and a mean size of ∼60 nm and their functionalization with poly(acrylic acid). The transverse magnetic relaxivity of both systems at 9.4 T is analyzed on the basis of magnetic susceptibility and magnetization measurements in order to evaluate their potential for application as high-field MRI contrast agents. In addition, the X-ray attenuation properties of these systems are also studied to determine their capabilities as computed tomography contrast agent. Finally, the colloidal stability under physiological pH conditions and the cytotoxicity of the functionalized NPs are also addressed to assess their suitability for bioimaging applications.

Enero, 2021 | DOI: 10.1021/acs.inorgchem.0c02601

Enhanced Directional Light Extraction from Patterned Rare-Earth Phosphor Films

Cabello-Olmo, E; Molet, P; Mihi, A; Lozano, G; Miguez, H
Advanced Optical Materials, 9 (2021) 2001611
Materiales Ópticos Multifuncionales


The combination of light‐emitting diodes (LEDs) and rare earth (RE) phosphors as color‐converting layers comprises the basis of solid‐state lighting. Indeed, most LED lamps include a photoluminescent coating made of phosphor material, i.e., crystalline matrix suitably doped with RE elements, to produce white light from a blue or ultraviolet LED chip. Transparent phosphor‐based films constitute starting materials for new refined emitters that allow different photonic designs to be implemented. Among the different photonic strategies typically employed to tune or enhance emission, surface texturing has proved its versatility and feasibility in a wide range of materials and devices. However, most of the nanofabrication techniques cannot be applied to RE phosphors directly because of their chemical stability or because of their cost. The first monolithic patterned structure of down‐shifting nanophosphors with square arrays of nanoholes with different lattice parameters is reported in this study. It is shown that a low‐cost soft‐nanolithography procedure can be applied to red‐emitting nanophosphors (GdVO4:Eu3+ nanocrystals) to tune their emission properties, attaining a twofold directional enhancement of the emitted light at predesigned emission wavelengths in specific directions.

Enero, 2021 | DOI: 10.1002/adom.202001611

Disentangling Electron–Phonon Coupling and Thermal Expansion Effects in the Band Gap Renormalization of Perovskite Nanocrystals

Rubino, A; Francisco-Lóprez, A.; Baker, A.J., Petrozza, A.; Calvo, M.E.; Goñi, A.R.; Míguez, H.
Journal of Physical Chemistry Letters, 12 (2021) 569-575
Materiales Ópticos Multifuncionales


The complex electron–phonon interaction occurring in bulk lead halide perovskites gives rise to anomalous temperature dependences, like the widening of the electronic band gap as temperature increases. However, possible confinement effects on the electron–phonon coupling in the nanocrystalline version of these materials remain unexplored. Herein, we study the temperature (ranging from 80 K to ambient) and hydrostatic pressure (from atmospheric to 0.6 GPa) dependence of the photoluminescence of ligand-free methylammonium lead triiodide nanocrystals with controlled sizes embedded in a porous silica matrix. This analysis allowed us to disentangle the effects of thermal expansion and electron–phonon interaction. As the crystallite size decreases, the electron–phonon contribution to the gap renormalization gains in importance. We provide a plausible explanation for this observation in terms of quantum confinement effects, showing that neither thermal expansion nor electron–phonon coupling effects may be disregarded when analyzing the temperature dependence of the optoelectronic properties of perovskite lead halide nanocrystals.

Enero, 2021 | DOI: 10.1021/acs.jpclett.0c03042

Critical Influence of the Processing Route on the Mechanical Properties of Zirconia Composites with Graphene Nanoplatelets

Gallardo-Lopez, A; Munoz-Ferreiro, C; Lopez-Pernia, C; Jimenez-Pique, E; Gutierrez-Mora, F; Morales-Rodriguez, A; Poyato, R
Materials, 14 (2021) 108
Reactividad de Sólidos


Graphene-based nanostructures, used as potential reinforcement in ceramic composites, have a great tendency to agglomerate. This requires the use of homogenization techniques during the powder processing, posing the need to evaluate how these techniques affect the microstructure and the mechanical properties of the resulting composites. The influence of the processing route on the properties of 3YTZP (3 mol % yttria tetragonal zirconia polycrystals) ceramic composites with 10 vol % cost-effective GNP (graphene nanoplatelets) has been addressed. Four different powder processing routines combining ultrasonic powder agitation (UA) and planetary ball milling (PBM) in wet and dry media have been used and all the composites were densified by spark plasma sintering (SPS). The mechanical properties at room temperature in the macroscale have been assessed by Vickers indentations, four-point bending tests and the impulse-echo technique, while instrumented indentation was used to measure the hardness and Young’s modulus at the nanoscale. The application of dry-PBM enhances greatly the mechanical and electrical isotropy of the composites, slightly increases the hardness and lowers the elastic modulus, independently of the application of UA. The combination of UA and dry-PBM enhances the flexure strength by 50%, which is desirable for structural applications.

Enero, 2021 | DOI: 10.3390/ma14010108

Sol-gel synthesis of ZnWO4-(ZnO) composite materials. Characterization and photocatalytic properties

Jaramillo-Páez, C., Navío, J.A., Puga, F., Hidalgo, M.C.
Journal of Photochemistry & Photobiology, A: Chemistry, 404 (2021) 112962
Fotocatálisis Heterogénea: Aplicaciones


ZnWO4 based powder photocatalyst have been successfully prepared by calcining a co-precipitated precursor (ZnWO) obtained from aqueous Zn2+ and WO4 2− solutions at pH = 7, without surfactants addition. The as-formed sample was characterized by XRD, N2-absorption, SEM, TEM, DRS and XPS. Both techniques, XRD and XPS results showed that prepared sample corresponds to a crystalline, Zn-enriched composition, ZnWO4 indicating the formation of a ZnWO4-(ZnO) composite, whit ca. 10 wt.-% of ZnO confirmed by XRF analysis. Photocatalytic activities towards degradation of Rhodamine B (RhB), Methyl Orange (MO) and Phenol, under UV-illumination, was investigated not only by monitoring the percentages of conversion of substrates, but also by estimating the corresponding percentages of mineralization that accompany the photocatalytic process. Comparative substrateconversion rates estimated per surface area unit of catalyst, showed that the activity for ZnWO4-(ZnO) composite is similar to that for TiO2(P25), at least for MO and RhB, and even higher that for TiO2(P25) in respect to phenol conversion. By adding TEA to the synthesis procedure, a composite named as ZnWO4-ZnO-(pH = 10)-600 is generated, which has a higher proportion of ZnO (ca. 39 %) and superior specific surface area than the so-called ZnWO4-(ZnO) sample. Furthermore, the photocatalytic degradation of MO using the former material indicates that it is superior to ZnWO4-(ZnO) and even that TiO2(P25) itself under the same operational conditions. 

Enero, 2021 | DOI: 10.1016/j.jphotochem.2020.112962

Physicochemical surface analysis and germination at different irrigation conditions of DBD plasma‐treated wheat seeds

Molina, R; Lalueza, A; Lopez-Santos, C; Ghobeira, R; Cools, P; Morent, R; de Geyter, N; Gonzalez-Elipe, AR
Plasma Processes and Polymers, (2020)
Nanotecnología en Superficies y Plasma


Plasma treatment is increasingly being explored as an effective presowing treatment improving seed germination. This study examines the synergetic effect of the irrigation condition and the physicochemical surface properties of wheat seeds subjected to atmospheric dielectric barrier discharge plasma activation on their water uptake and germination. Extensive surface analysis revealed a remarkably enhanced wettability of plasma-treated seeds due to the insertion of oxygen-containing functionalities on their surface. However, long plasma exposures damaged the outermost layers of the pericarp due to a pronounced oxidative etching effect. Although the seed germination capacity was not affected by the plasma treatments, short plasma exposures were shown to enhance water uptake and accelerate seed germination, especially under water-scarcity conditions.

Enero, 2021 | DOI: 10.1002/ppap.202000086

Sponge-like processed D-periodic self-assembled atelocollagen supports bone formation in vivo

Borrego-Gonzalez, S; Rico-Llanos, G; Becerra, J; Diaz-Cuenca, A; Visser, R
Materials Science & Engineering C-Materials for Biological Applications, 120 (2021) art.111679
Materiales para Bioingeniería y Regeneración Tisular


Fibrous biopolymeric collagen extracted from animal tissues has been widely used for fabricating matrices for bone tissue engineering (BTE). However, animal extracted collagens can trigger immune reactions when implanted in vivo and the presence of native crosslinks leads to batch-to-batch variability. Atelocollagen, a monomeric form of collagen, is free of telopeptides, which are mainly responsible for the immunogenicity of collagen, and can self-assemble in vitro to obtain fibrils with the characteristic D-periodic staining pattern of native collagen. However, atelocollagen-based biomaterials have not extensively been studied and, hence, their suitability for BTE remains relatively unexplored. Besides, to stabilize collagen biomaterials, chemical and physical crosslinking are used, although chemical agents are cytotoxic while the physical methods yield a less effective crosslinking. A combination of physical and chemical crosslinking is a suitable alternative that has rarely been tested in BTE programs. In this work, a sponge-like biomaterial (DCol-S) was processed from D-periodic self-assembled atelocollagen and its stabilization was studied using the combination of a dehydrothermal treatment (DHT) and minimal glutaraldehyde (GTA) exposition crosslinking, to increase the resistance to degradation of the scaffold without a major effect on the biomaterial structure. The microstructural features of the final sponges were characterised and compared to a commercial biomaterial processed from native bovine collagen (Helistat (R), Integra Lifesciences, NJ, USA), demonstrating that a D-periodic nanostructure was obtained and maintained after processing of the sponges. MC3T3-E1 preosteoblast adhesion, proliferation and differentiation assays in vitro showed that DCol-S is biocompatible. Furthermore, intramuscular implantation of the biomaterials loaded with rhBMP-2 revealed that the double-crosslinked sponges were able to support ectopic bone formation, while sponges stabilised only with the DHT treatment were not. Altogether, these findings show that atelocollagen-based sponges stabilised with a DHT treatment followed by a mild GTA crosslinking are a suitable alternative to polymeric extracted collagen for BTE applications.

Enero, 2021 | DOI: 10.1016/j.msec.2020.111679

Photocatalytic activity of ZnO nanoparticles and the role of the synthesis method on their physical and chemical properties

Uribe-Lopez, MC; Hidalgo-Lopez, MC; Lopez-Gonzalez, R; Frias-Marquez, DM; Nunez-Nogueira, G; Hernandez-Castillo, D; Alvarez-Lemus, MA
Journal of Photochemistry & Photobiology, A: Chemistry, 404 (2021) 112866
Fotocatálisis Heterogénea: Aplicaciones


In the present study, we report on the effect of the synthesis method in the photoactivity of ZnO-NPs. The nanoparticles were prepared by precipitation and sol-gel procedures using zinc nitrate and zinc (II) acetylacetonate as ZnO precursors, respectively. The obtained samples were named as ZnO-PP (precipitation method) and ZnO-SG (sol-gel method). The powders were calcined at 500 degrees C and further characterized by Fourier Transform Infrared spectroscopy, X-ray Powder Diffraction, N-2 adsorption, thermal analysis, Diffuse Reflectance UV-Vis spectroscopy, and Electron Microscopy. Both methods of synthesis lead to formation of pure ZnO with hexagonal-wurtzite crystalline structures with average crystallite sizes similar to 30 nm. The specific surface area was affected by the synthesis method, since SBET values were 5 m(2)/g and 13 m(2)/g for sol-gel and precipitation method, respectively. The electron microscopy revealed significant changes in morphology for the obtained nanoparticles, as sol-gel directed the hexagonal rod-like geometries (similar to 50 nm in diameter) while quasi-spherical nanoparticles (similar to 100 nm in diameter) were formed using precipitation method. Photocatalytic activity was estimated by degrading phenol (50 ppm) as probe molecule under UVA irradiation (lambda = 356 nm), the results demonstrated that ZnO-PP reached 100 % of degradation after 120 min and 90 % of the pollutant was mineralized, whereas for ZnO-SG the results were 80 % and 48 % respectively. Fluorescence test using terephthalic acid (TA) demonstrated higher formation of OH center dot radicals for ZnO synthesized by precipitation method, which could explain the higher photodegradation and mineralization observed. These results support that even slight differences in physical and chemical properties of ZnO, have a significant impact on the photocatalytic performance of such nanoparticles.

Enero, 2021 | DOI: 10.1016/j.jphotochem.2020.112866

Elucidating the Promotional Effect of Cerium in the Dry Reforming of Methane

Rodriguez-Gomez, A; Lopez-Martin, A; Ramirez, A; Gascon, J; Caballero, A
Chemcatchem, 13 (2021) 553-563
Materiales y Procesos Catalíticos de Interés Ambiental y Energético


A series of Ni-Ce catalysts supported on SBA-15 has been prepared by co-impregnation, extensively characterized and evaluated in the carbon dioxide reforming of methane (DRM). The characterization by TEM, XRD and TPR has allowed us to determine the effect of metal loading on metal dispersion. Cerium was found to improve nickel location inside the mesopores of SBA-15 and to suppress coke formation during the DRM reaction. The analysis by XPS allowed us to associate the high cerium dispersion with the presence of low-coordinated Ce3+ sites, being main responsible for its promotional effect. A combination of XAS and XPS has permitted us to determine the physicochemical properties of metals under reduction conditions. The low nickel coordination number determined by XAS in N-Ce doped systems after reduction suggests the generation of very small nickel particles which showed greater catalytic activity and stability in the reaction, and a remarkable resistance to coke formation.

Enero, 2021 | DOI: 10.1002/cctc.202001527


Characterization, thermal and ceramic properties of phyllite clays from southeast Spain

Garzon, Eduardo; Perez-Villarejo, Luis; Sanchez-Soto, Pedro J.
Journal of Thermal Analysis and Calorimetry, 142 (2020) 1659-1670
Materiales Avanzados


The present research studied a set of phyllite clays from several deposits in southeast Spain. These phyllite clays have traditionally been used as sealing material to impermeabilize roofs, embankments, ponds, construction and waste landfill, with recent applications in the preparation of new mortars. However, studies on thermal behaviour and ceramic properties of phyllite clays have been scarce. The present research showed a summary of previous characterization studies on representative phyllite clays from these deposits with additional results. Mineralogical, by X-ray diffraction, and chemical, by X-ray fluorescence characterization of these samples were summarized. Thermal analysis methods (DTA-TG and thermal diffractometry) were applied to achieve a more complete mineralogical characterization. Several phyllite clay samples were selected for a ceramic study by firing pressed powdered samples up to 1300 degrees C. Sintered or vitrified materials, with porosities almost zero, were obtained from these phyllite clays after firing at 1100-1200 degrees C, with apparent densities between 2.1 and 2.4 g cm(-3). Higher firing temperatures (> 1250 degrees C) produced deformation and expansion of the ceramic bodies. These results allowed obtain the vitrification temperature (T-v) and the temperature of the maximum bulk density (T-d). According to the previous mineralogical and chemical characterization and the values of these parameters, the phyllite clay samples were classified in three varieties, as follows: (1)Micaceous, characterized by predominant layer silicates, mainly muscovite or illite, alkaline elements (mainly K2O higher than 3.5 mass%) and lower values of both T(v)and T-d, (2)Quartzitic, with predominant quartz and SiO(2)and intermediate values of T(v)and T-d, and (3)Carbonaceous, characterized by predominant dolomite, medium contents of CaO and MgO and higher values of both T(v)and T-d. These results are interesting for the application of these phyllite clays as ceramic raw materials.

Diciembre, 2020 | DOI: 10.1007/s10973-020-10160-9

Robust anti-icing superhydrophobic aluminum alloy surfaces by grafting fluorocarbon molecular chains

Rico, V; Mora, J; Garcia, P; Aguero, A; Borras, A; Gonzalez-Elipe, AR; Lopez-Santos, C
Applied Materials Today, 21 (2020) 100815
Nanotecnología en Superficies y Plasma


Infusion of low surface tension liquids in nanostructured surfaces is currently used to promote an anti icing response, although the long term stability of these systems is often jeopardized by losses of the infused liquid. In this work, we propose an alternative to the infusion procedure to induce a more effective and long lasting anti-icing capacity. The method consists of a combination of surface nanostructuration with the chemical grafting of fluorocarbon molecules. Al6061 substrates have been subjected to laser roughening and further modified with a nanostructured Al2O3 thin film to achieve a dual roughness and porous surface state. These surfaces have been subjected to a grafting treatment with perfluorooctyltriethoxysilane (PFOTES) vapor or, for comparative purposes, infused with a low surface tension liquid. A comparative analysis of the wetting, water condensation and anti-icing properties of these two systems showed an outstandingly better performance for the grafted surfaces with respect to the infused ones. Grafted surfaces were markedly superhydrophobic and required higher water vapor pressures to induce condensation. When looking for their anti-icing capacity, they presented quite long freezing delay times for supercooled water droplets (i.e. almost four hours) and exhibited a notably low ice accretion in a wind tunnel test. The high aging resistance and durability of these grafted surfaces and the reproducibility of the results obtained when subjected to successive ice accretion cycles show that molecular grafting is an efficient anti-icing methodology that, in aggressive media, may outperform the classical infusion procedures. The role of the fluorocarbon chains anchored on the surface in inducing an anti-icing functionality is discussed.

Diciembre, 2020 | DOI: 10.1016/j.apmt.2020.100815

(NH4)4[NiMo6O24H6].5H2O / g-C3N4 materials for selective photo-oxidation of Csingle bondO and Cdouble bondC bonds

Caudillo-Flores, U; Ansari, F; Bachiller-Baeza, B; Colon, G; Fernandez-Garcia, M; Kubacka, A
Applied Catalysis B-Environmental, 278 (2020) 119299
Materiales y Procesos Catalíticos de Interés Ambiental y Energético


Novel composite photo-catalysts having (NH4)(4)[NiMo6O24H6]center dot 5H(2)O Polyoxometalate (POM) species deposited over g-C3N4 are synthesized. Materials were characterized through a multitechnique approach showing the stability of the carbon nitride component both through the synthesis process and under reaction. Contrarily, the POM component evolves under reaction conditions to maximize the interaction with the support. Such a behavior renders, as measured by the quantum efficiency, highly active photo-catalysts in the photo-oxidation of 2-propanol and styrene both under UV and sunlight illumination, setting up the basis for a green catalytic process. The material having a 4 wt. % POM showed improved activity with respect to both parent constituents but also higher selectivity to the partial oxidation of the alcohol and the aromatic hydrocarbon to generate added value chemical compounds. A multitechnique approach investigating charge carrier fate demonstrates the key role played by the interaction between components to promote activity and selectivity in selective oxidation reactions.

Diciembre, 2020 | DOI: 10.1016/j.apcatb.2020.119299

Influence of Water on the Oxidation of NO on Pd/TiO2 Photocatalysts

M.J. Hernández Rodríguez; E. Pulido Melián; J. Araña; J.A. Navío; O.M. González Díaz; Dunia E. Santiago; J.M. Doña Rodríguez
Nanomaterials, 10 (2020) 2354
Fotocatálisis Heterogénea: Aplicaciones


Two series of new photocatalysts were synthesized based on modification with Pd of the commercial P25 photocatalyst (EVONIK®). Two techniques were employed to incorporate Pd nanoparticles on the P25 surface: photodeposition (series Pd-P) and impregnation (series Pd-I). Both series were characterized in depth using a variety of instrumental techniques: BET, DRS, XRD, XPS, TEM, FTIR and FESEM. The modified series exhibited a significant change in pore size distribution, but no differences compared to the original P25 with respect to crystalline phase ratio or particle size were observed. The Pd0 oxidation state was predominant in the Pd-P series, while the presence of the Pd2+ oxidation state was additionally observed in the Pd-I series. The photoactivity tests were performed in a continuous photoreactor with the photocatalysts deposited, by dip-coating, on borosilicate glass plates. A total of 500 ppb of NO was used as input flow at a volumetric flow rate of 1.2 L·min−1, and different relative humidities from 0 to 65% were tested. The results obtained show that under UV-vis or Vis radiation, the presence of Pd nanoparticles favors NO removal independently of the Pd incorporation method employed and independently of the tested relative humidity conditions. This improvement seems to be related to the different interaction of the water with the surface of the photocatalysts in the presence or absence of Pd. It was found in the catalyst without Pd that disproportionation of NO2 is favored through its reaction with water, with faster surface saturation. In contrast, in the catalysts with Pd, disproportionation took place through nitro-chelates and adsorbed NO2 formed from the photocatalytic oxidation of the NO. This different mechanism explains the greater efficiency in NOx removal in the catalysts with Pd. Comparing the two series of catalysts with Pd, Pd-P and Pd-I, greater activity of the Pd-P series was observed under both UV-vis and Vis radiation. It was shown that the Pd0 oxidation state is responsible for this greater activity as the Pd-I series improves its activity in successive cycles due to a reduction in Pd2+ species during the photoactivity tests.

Diciembre, 2020 | DOI: 10.3390/nano10122354