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An insight on the design of mercapto functionalized swelling brittle micas

Osuna, FJ; Pavon, E; Alba, MD
Journal of Colloid and Interface Science, 561 (2020) 533-541


Surface modification of natural clay minerals with reagents containing metal chelating groups has great environmental value. The functionalization by adsorption or grafting guarantees a durable immobilization of the reactive organic groups, preventing their leaching when they are used in liquid media. The aim of this research was the designed mercapto functionalization of swelling brittle micas, Na-Mn, thorough both chemical and physical mechanisms. Na-Mn were functionalized with 2-mercaptoethylammonium (MEA), 2,3-dimercapto-1-propanol (BAL) and (3-mercaptopropyl)trimethoxysilane (MPTMS). The thiol concentration on swelling brittle micas is higher than the observed value for others adsorbents. The cation exchange reaction with MEA and one-step grafting with MPTMS in acid medium are the most efficient mercapto functionalization mechanism.

March, 2020 | DOI: 10.1016/j.jcis.2019.11.028

Preparation of ZnFe2O4/ZnO composite: Effect of operational parameters for photocatalytic degradation of dyes under UV and visible illumination

Zouhier, M.; Tanji, K.; Navio, J.A.; Hidalgo, M.C.; Jaramillo-Páez, C.; Kherbeche, A.
Journal of Photochemistry and Photobiology A: Chemistry, 390 (2020) 112305


An ZnFe2O4/ZnO composite catalyst was prepared by solution combustion method. In this study, one nominal molar percentage of iron was used in the synthesis, corresponding to 20 % molar relative to ZnO. The samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray Fluorescence (XRF), Scanning Electronic Microscopy (SEM), Transmission Electronic Microscopy (TEM) and Ultraviolet-visible (UV–vis) diffuse spectroscopy (DRS). The photocatalytic activities of the catalysts were investigated based on the degradation of two dyes, methylene blue (MB) and remazol brilliant blue (RBB), in aqueous solution under both UV and visible light illumination respectively. It was found that the composite had a good photocatalytic activity at basic pH by using 1 g/L of catalyst under UV illumination for both MB and RBB. Under visible illumination, while pristine ZnO showed no activity, the composite exhibited an excellent visible efficiency, reaching up to an 80 % conversion of the initial dye concentrations in 2 h. The enhancement of the visible photocatalytic activity of Fe/ZnO sample with respect to pristine ZnO is attributed to the formation of ZnFe2O4 coupled with ZnO, having a narrow band gap value that contributes to the absorption of visible photons with an improved separation path for the photo-generated carriers.

March, 2020 | DOI: 10.1016/j.jphotochem.2019.112305

Localized surface plasmon effects on the photophysics of perovskite thin films embedding metal nanoparticles

Bayles, A; Carretero-Palacios, S; Calio, L; Lozano, G; Calvo, ME; Miguez, H
Journal of Materials Chemistry C, 8 (2020) 916-921


Herein we provide direct experimental evidence that proves that the photophysical properties of thin methylammonium lead iodide perovskite films are significantly enhanced by localized surface plasmon resonances (SPRs). Observations are well supported by rigorous calculations that prove that improved light harvesting can be unequivocally attributed to plasmonic scattering and near field reinforcement effects around silver nanoparticles embedded within the semiconductor layer. Adequate design of the localized SPR allows raising the absorptance of a 300 nm thick film at well-defined spectral regions while minimizing the parasitic absorption from the metallic inclusions. Measured enhancements can be as large as 80% at specific wavelengths and 20% when integrated over the whole range at which SPR occurs, in agreement with theoretical estimations. Simultaneously, the characteristic quenching effect that the vicinity of metals has on the photoluminescence of semiconductors is largely compensated for by the combined effect of the enhanced photoexcitation and the higher local density of photon states occurring at SPR frequencies, with a two fold increase of the perovskite photoemission efficiency being measured.

March, 2020 | DOI: 10.1039/c9tc05785d

Positron annihilation analysis of nanopores and growth mechanism of oblique angle evaporated TiO2 and SiO2 thin films and multilayers

Garcia-Valenzuela, A; Butterling, M; Liedke, MO; Hirschmann, E; Trinh, TT; Attallah, AG; Wagner, A; Alvarez, R; Gil-Rostra, J; Rico, V; Palmero, A; Gonzalez-Elipe, AR
Microporous and Mesoporous Materials, 295 (2020) 109968


The nano-porosity embedded into the tilted and separated nanocolumns characteristic of the microstructure of evaporated thin films at oblique angles has been critically assessed by various variants of the positron annihilation spectroscopy. This technique represents a powerful tool for the analysis of porosity, defects and internal interfaces of materials, and has been applied to different as-deposited SiO2 and TiO2 thin films as well as SiO2/TiO2 multilayers prepared by electron beam evaporation at 70 and 85 zenithal angles. It is shown that, under same deposition conditions, the concentration of internal nano-pores in SiO2 is higher than in TiO2 nanocolumns, while the situation is closer to this latter in TiO2/SiO2 multilayers. These features have been compared with the predictions of a Monte Carlo simulation of the film growth and explained by considering the influence of the chemical composition on the growth mechanism and, ultimately, on the structure of the films.

March, 2020 | DOI: 10.1016/j.micromeso.2019.109968

Pt–TiO2–Nb2O5 heterojunction as effective photocatalyst for the degradation of diclofenac and ketoprofen

Sacco, O.l; Murcia, J.J.; Lara, A.E.; Hernández-Laverde, M.; Rojas, H.; Navío, J.A.; Hidalgo, M.C.; Vaiano, V.
Materials Science in Semiconductor Processing, 107 (2020) 104839


Pt–TiO2–Nb2O5 heterojunction was synthetized and studied for the photocatalytic removal of diclofenac (DCF) and ketoprofen (KTF) under UV light irradiation. The physical-chemical properties of the prepared catalysts were analysed by different characterization techniques revealing that the lowest platinum nanoparticle size and the better metal distribution was observed in Pt–TiO2–Nb2O5 sample. The Pt–TiO2–Nb2O5 heterojunction possessed the best photocatalytic activity toward both the photodegradation and mineralization of the two selected pollutants. The optimal photocatalyst showed a DCF and KTF mineralization rate of 0.0555 and 0.0746 min−1, respectively, which were higher than those of Pt–TiO2 (0.0321 min−1 for DCF and 0.0597 min−1 for KTF). The experiments driven to analyse the effects of free radical capture showed that ·OH, ·O2− and h+ have a primary role in reactive during the photocatalytic reaction. The improved photocatalytic performances of the Pt–TiO2–Nb2O5 heterojunction could be argue by a direct Z-scheme mechanism in which the Pt0 nanoparticles could act as a bridge between TiO2 and Nb2O5, improving the electron-hole separation and, ultimately, enhancing the photocatalytic removal rate of both DCF and KTF.

March, 2020 | DOI: 10.1016/j.mssp.2019.104839

Robust label-free CuxCoyOz electrochemical sensors for hexose detection during fermentation process monitoring

Lopez-Fernandez, E; Gil-Rostra, J; Espinos, JP; Gonzalez, R; Yubero, F; de Lucas-Consuegra, A; Gonzalez-Elipe, AR
Sensors and Actuators B-Chemical, 304 (2020) 127360


Label free electrochemical sensors of glucose are used whenever long-term operation and stable response are required. For this purpose, various metals and oxides of the first transition series have been proposed as alternative to more expensive noble metal electrochemical sensors. In this work we propose a new formulation consisting of copper-cobalt mixed oxides which, in the form of porous and nanostructured thin films with well controlled Co/Cu ratio, are prepared at room temperature in one step by a modification of the magnetron sputtering oblique angle deposition procedure. Films with various compositions were electrochemically characterized by cyclic voltammetry to determine their amperometric response to glucose as a function of voltage and NaOH electrolyte concentration. This analysis showed that films with a Co/Cu atomic ratio equal 3.4 presented a maximum sensitivity (0.710 A M−1 cm−2), a small limit of detection (0.105 μM) and a resilient behaviour upon cycling operation and long storage periods that clearly overpassed the performance of copper and cobalt single oxides. The CuxCoyO electrocatalysts also presented a good selectivity towards glucose and fructose in the presence of common interference compounds found in biological fluids (e.g., ascorbic acid, acetaminophen and uric acid), sucrose and ethanol, this latter present in many agrofood liquids. The possibilities of this sensor electrocatalyst have been tested for the analysis of a wine synthetic fermentation process. The comparison of the electrochemical results with conventional analytical methods showed a lineal amperometric response with respect hexose contents in a must at different stages of its transformation into wine.

February, 2020 | DOI: 10.1016/j.snb.2019.127360

Role of Fe(III) in aqueous solution or deposited on ZnO surface in the photoassisted degradation of rhodamine B and caffeine

Tanji, Karim; Navio, J A; Martin-Gomez, A N; Hidalgo, M C; Jaramillo-Paez, C; Naja, Jamal; Hassoune, Hicham; Kherbeche, Abdelhak
Chemosphere, 241 (2020) 125009


Iron (III) was incorporated, to the surface of a synthesized ZnO, using two nominal molar percentages of Fe (III): 1% and 5% Fe relative to ZnO. Samples dried and calcined at 200 °C and 400 °C for 2 h, were characterized by XRD, XPS, XRF, N2-adsorption-BET and (UV–vis)-DRS. Photocatalytic activities of the catalysts were assessed based on the degradation of rhodamine B (RhB) and caffeine (CAF) in aqueous solution under two irradiation conditions: UV and visible light illumination. Prior to the photocatalytic tests, the interaction of each one of the substrates with either Fe(III) or Fe(II) was studied in homogeneous medium under UV-illumination and oxygenated environment. It was found that Fe (III) can play an important role in homogeneous media in the photoassisted degradation, both of rhodamine B and caffeine, while Fe (II) does not exert a relevant role in the photoassisted degradation of the referred substrates. Fe–ZnO samples display similar or poorer performance than pure ZnO in the presence of UV light for both studied substrates. The phenomenon can be attributed to the formation of either goethite or ZnFe2O4 at the ZnO surface where the coupled Fe3+/Fe2+ can act as recombination centers for the photogenerated charges. On the contrary, all Fe–ZnO samples showed enhanced photocatalytic activity under visible illumination which seems to be independent of the iron content. In this context, the mechanisms for photoassisted degradation of both the substrates in homogeneous medium and photocatalytic degradation are discussed, as well as the role of Fe in the photodegradation processes.

February, 2020 | DOI: 10.1016/j.chemosphere.2019.125009

Synthesis of Mn2+-doped ZnS by a mechanically induced self-sustaining reaction

Aviles, MA; Cordoba, JM; Sayagues, MJ; Gotor, FJ
Journal of Materials Science, 55 (2020) 1603-1613


The mechanochemical process denoted as a mechanically induced self-sustaining reaction was successfully applied in obtaining Mn-doped ZnS samples with Mn content between 0 and 5 mol%. The process consists in milling Zn/Mn/S powder elemental mixtures with the appropriate stoichiometry, which promotes after approximately 80 min the induction of a combustion reaction. The doping level was properly adjusted by controlling the atomic ratio of the starting mixture. A complete characterization of samples was carried out, including X-ray diffraction, high-resolution transmission electron microscopy, selected area electron diffraction, energy-dispersive X-ray spectroscopy, Raman spectroscopy, diffuse reflectance UV-Vis spectroscopy and emission and excitation photoluminescence measurements. A wurtzite structure, in which Mn2+ replaces Zn2+, was obtained with a nanometric character. The photoluminescence of samples showed the characteristic (Mn2+T1)-T-4-(6)A(1) emission that was highly dependent on the doping level. The maximum luminescence efficiency through the ZnS excitation was found for a doping value of 1 mol%. The photoluminescence showed virtually no contribution from the host emission, which confirmed that samples were properly doped.

February, 2020 | DOI: 10.1007/s10853-019-04138-8

Hybrid ZnO/Ag3PO4 photocatalysts, with low and high phosphate molar percentages

Martín-Gómez, A.N.;Navío, J.A.;Jaramillo-Páeza, C.;Sánchez-Cid, P.;Hidalgo, M.C.
Journal of Photochemistry and Photobiology A: Chemistry, (2019) 112196


In this work, a previously optimized synthesized ZnO photocatalyst was modified with different molar percentages of Ag3PO4 through a facile in situ precipitation–deposition method and then characterized by different techniques (XRD, XRF, BET, UV–vis DRS, SEM, TEM and XPS). The incorporation of Ag3PO4 produces important changes in the light absorption properties with a significant absorbance in the visible region observed for ZnO modified with different amounts of Ag3PO4; the optical absorption intensity in the visible region of the coupled ZnO/Ag3PO4 increases as the molar percentages of Ag3PO4 increases, evidencing a clear dependence on the content of Ag3PO4. However, this work shows that the incorporation of Ag3PO4 in almost all cases reduces the photocatalytic capacity of ZnO, except when it is used in a specific percentage of 10 % and only being more active against rhodamine B and not on the Caffeine. SEM images and elemental mapping indicate that Ag3PO4 disperses very well in the ZnO particles, exhibiting an almost homogeneous distribution, showing zones with cumulus of Ag3PO4 (rich in P-Ag) in contact with ZnO-zones (rich in Zn). All the prepared photocatalysts were tested in the photocatalytic degradation of rhodamine B as a dye, and caffeine as a toxic and persistent emerging compound under UV and visible light illumination. It is reported that not only the ZnO:Ag3PO4 ratio is an important factor that influences the photocatalytic process of substrate degradation, but also the nature of the substrate has an important influence on the photocatalytic behavior of the materials under both UV and visible illumination. Thus, pristine Ag3PO4 showed high photocatalytic degradation for rhodamine B, while for caffeine negligible photocatalytic degradation was found in both the UV and visible regions. The thermal- and photo-stability of the coupled system was also studied. At least, for rhodamine B no loss of photocatalytic activity has been observed after five recycles although the mineralization degree progressively diminished along the recycles.

February, 2020 | DOI: 10.1016/j.jphotochem.2019.112196

Influence of DSC thermal lag on evaluation of crystallization kinetics

Svoboda, R; Maqueda, LP; Podzemna, V; Perejon, A; Svoboda, O
Journal of Non-Crystalline Solids, 528 (2020) 119738


Influence of added thermal resistance on crystallization kinetics, as measured by differential scanning calorimetry (DSC), of the Se70Te30 glass was studied. The increase of thermal resistance was achieved by adding polytetrafluorethylene discs of different thicknesses (up to 0.5 mm) in-between the DSC platform and the pan with sample. Increase of the thermal resistance led to an apparent decrease (by more than 30%) in the crystallization enthalpy. Significant change of model-free kinetics occurred: apparent activation energy E of the crystallization process decreased (by more than 20%) due to the DSC data being progressively shifted to higher temperatures with increasing heating rate. The model-based kinetics was changed only slightly; the DSC peaks retained their asymmetry and the choice of the appropriate model was not influenced by the added thermal resistance. The temperature shift caused by added thermal lag was modeled for the low-to-moderate heating rates.

January, 2020 | DOI: 10.1016/j.jnoncrysol.2019.119738

Enhanced Stability of Perovskite Solar Cells Incorporating Dopant-Free Crystalline Spiro-OMeTAD Layers by Vacuum Sublimation

Barranco, A; Lopez-Santos, MC; Idigoras, J; Aparicio, FJ; Obrero-Perez, J; Lopez-Flores, V; Contreras-Bernal, L; Rico, V; Ferrer, J; Espinos, JP; Borras, A; Anta, JA; Sanchez-Valencia, JR
Advanced Energy Materials, (2020) 1901524


The main handicap still hindering the eventual exploitation of organometal halide perovskite-based solar cells is their poor stability under prolonged illumination, ambient conditions, and increased temperatures. This article shows for the first time the vacuum processing of the most widely used solid-state hole conductor (SSHC), i.e., the Spiro-OMeTAD [2,2 ',7,7 '-tetrakis (N,N-di-p-methoxyphenyl-amine) 9,9 '-spirobifluorene], and how its dopant-free crystalline formation unprecedently improves perovskite solar cell (PSC) stability under continuous illumination by about two orders of magnitude with respect to the solution-processed reference and after annealing in air up to 200 degrees C. It is demonstrated that the control over the temperature of the samples during the vacuum deposition enhances the crystallinity of the SSHC, obtaining a preferential orientation along the pi-pi stacking direction. These results may represent a milestone toward the full vacuum processing of hybrid organic halide PSCs as well as light-emitting diodes, with promising impacts on the development of durable devices. The microstructure, purity, and crystallinity of the vacuum sublimated Spiro-OMeTAD layers are fully elucidated by applying an unparalleled set of complementary characterization techniques, including scanning electron microscopy, X-ray diffraction, grazing-incidence small-angle X-ray scattering and grazing-incidence wide-angle X-ray scattering, X-ray photoelectron spectroscopy, and Rutherford backscattering spectroscopy.

January, 2020 | DOI: 10.1002/aenm.201901524

Low gas consumption fabrication of He-3 solid targets for nuclear reactions

Fernandez, A; Hufschmidt, D; Colaux, JL; Valiente-Dobon, JJ; Godinho, V; de Haro, MCJ; Feria, D; Gadea, A; Lucas, S
Materials & Design, 186 (2020) 108337


Nanoporous solids that stabilize trapped gas nanobubbles open new possibilities to fabricate solid targets for nuclear reactions. A methodology is described based on the magnetron sputtering (MS) technique operated under quasistatic flux conditions to produce such nanocomposites films with He-3 contents of up to 16 at.% in an amorphous-silicon matrix. In addition to the characteristic low pressure (3-6 Pa) needed for the gas discharge, the method ensures almost complete reduction of the process gas flow during film fabrication. The method could produce similar materials to those obtained under classical dynamic flux conditions for MS. The drastic reduction (>99.5%) of the gas consumption is fundamental for the fabrication of targets with scarce and expensive gases. Si:He-3 and W:He-3 targets are presented together with their microstructural (scanning and transmission electron microscopy, SEM and TEM respectively) and compositional (Ion Beam Analysis, IBA) characterization. The He-3 content achieved was over 1 x 10(18) at/cm(2) for film thicknesses between 1.5 and 3 mu m for both Si and W matrices. First experiments to probe the stability of the targets for nuclear reaction studies in inverse kinematics configurations are presented. 

January, 2020 | DOI: 10.1016/j.matdes.2019.108337

Tribomechanical properties of hard Cr-doped DLC coatings deposited by low-frequency HiPIMS

Santiago, JA; Fernandez-Martinez, I; Sanchez-Lopez, JC; Rojas, TC; Wennberg, A; Bellido-Gonzalez, V; Molina-Aldareguia, JM; Monclus, MA; Gonzalez-Arrabal, R
Surface & Coatings Technology, 382 (2020) 124899


Cr-doped diamond-like carbon (Cr-DLC) films with Cr contents ranging from 3 up to 20 at. % were synthesised in a codeposition process with HiPIMS (Cr deposition) and DC-pulsed technology (C deposition). The application of HiPIMS at low frequencies was observed to significantly enhance the energy density during the Cr plasma discharge due to the interaction of Cr-C species. The higher energy bombardment at low HiPIMS frequencies allowed doping with Cr the DLC structure avoiding the graphitization of the carbon structure. EELS spectroscopy was used to evaluate sp(3) content and Raman was used for sp(2) structural characterization of the films. Enhanced mechanical properties (hardness up to 30 GPa) were observed with nanoindentation for Cr-doped DLC at low frequencies. High temperature nanoindentation tests were also performed from room temperature to 425 degrees C in order to evaluate the evolution of hardness and Young Modulus with temperature. The results showed that the mechanical properties at high temperature mainly depend on the initial sp(3)-sp(2) structure. Tribological tests were carried out in air from room temperature to 250 degrees C. Cr-doped DLC coatings deposited by low-frequency HiPIMS showed lower friction and wear compared to undoped DLC.

January, 2020 | DOI: 10.1016/j.surfcoat.2019.124899

Dipole reorientation and local density of optical states influence the emission of light-emitting electrochemical cells

Jimenez-Solano, Alberto; Martinez-Sarti, Laura; Pertegas, Antonio; Lozano, Gabriel; Bolink, Henk J; Miguez, Hernan
Physical Chemistry Chemical Physics


Herein, we analyze the temporal evolution of the electroluminescence of light-emitting electrochemical cells (LECs), a thin-film light-emitting device, in order to maximize the luminous power radiated by these devices. A careful analysis of the spectral and angular distribution of the emission of LECs fabricated under the same experimental conditions allows describing the dynamics of the spatial region from which LECs emit, i.e. the generation zone, as bias is applied. This effect is mediated by dipole reorientation within such an emissive region and its optical environment, since its spatial drift yields a different interplay between the intrinsic emission of the emitters and the local density of optical states of the system. Our results demonstrate that engineering the optical environment in thin-film light-emitting devices is key to maximize their brightness.

January, 2020 | DOI: 10.1039/c9cp05505c

Development of Ti(C,N)-based cermets with (Co,Fe,Ni)-based high entropy alloys as binder phase

de la Obra, AG; Sayagues, MJ; Chicardi, E; Gotor, FJ
Journal of Alloys and Compounds, 814 (2020) 152218


High entropy alloys have been proposed as novel binder phases in cemented carbides and cermets. Many aspects related to the stability of these alloys during the liquid phase sintering process are still unclear and were addressed in this work. Consolidated Ti(C,N)-based cermets using four different (Co,Fe,Ni)based high entropy alloys as the binder phase were obtained. The chosen alloys - CoCrCuFeNi, CoCrFeNiV, CoCrFeMnNi and CoFeMnNiV - were previously synthesized through mechanical alloying and a single alloyed solid solution phase with fcc structure and nanometric character was always obtained. The powdered alloys and the consolidated cermets were analyzed by X-ray diffraction, scanning electron microscopy, X-ray energy dispersive spectrometry and transmission electron microscopy. Differential thermal analysis was employed to determine the melting point of the four high entropy alloys that ranged between 1310 degrees C and 1375 degrees C. Although a high temperature of 1575 degrees C was required to obtain the highest cermet densification by pressureless sintering, porosity still remained in most of the cermets. Best densification was achieved when CoCrFeNiV was used as the binder phase. During liquid phase sintering, different compositional changes were observed in the ceramic and binder phases. A core-rim microstructure was observed in cermets containing V in the alloys (CoCrFeNiV and CoFeMnNiV), since this element was incorporated to the carbonitride structure during sintering. A slight Cr segregation was detected in cermets containing Cr, leading to CrTi-rich alloys in small binder regions. However, a great Cu segregation was produced when CoCrCuFeNi was used, and the formation of two different fcc alloys -a Cu-rich and a Cu-depleted- was observed. Finally, a loss of Mn was also evidenced in CoCrFeMnNi and CoFeMnNiV, probably due to its sublimation at the sintering temperature. 

January, 2020 | DOI: 10.1016/j.jallcom.2019.152218

Effect of synthesis pH on the physicochemical properties of a synthesized Bi2WO6 and the type of substrate chosen, in assessing its photo-catalytic activities

Jaramillo-Páez, C.; Navío, J.A.; Hidalgo, M.C.
Arabian Journal of Chemistry, 13 (2020) 431-443


Crystalline orthorhombic Bi2WO6 powders were synthesized by a hydrothermal method from aqueous solutions of Bi(NO3)35H2O and Na2WO42H2O over a range of three selected pH values (2.0, 5.0 and 7.0), using NaOH as precipitating agent. The as-prepared catalysts were characterized by XRD, BET, FE-SEM, TEM, XPS and UV-vis spectroscopy. The effect of pH-synthesis on crystallinity,  morphologies, surface area and optical absorption properties, were investigated.
Although the pH has a marked influence on morphology, the nature of the precipitating agent (NaOH or TEA) also influences the morphology and surface structure composition, as it is observed in the present work. Three different probe molecules were used to evaluate the photocatalytic properties under two illumination conditions (UV and Visible): Methyl Orange and Rhodamine B were chosen as dye substrates and Phenol as a transparent substrate. The photo-catalytic activities are strongly dependent not only on the pH used in the synthesis but also on the nature of the chosen substrate in assessing the photo-catalytic activities. Results were compared with those obtained when using TiO2(P25, Evonik) in the same experimental conditions. The photocatalytic activity of one of the synthesised samples has been evaluated by exposing a mixture of Rhodamine B and Phenol in water, to different illumination conditions. Our results provide new evidences about the issue of whether dyes are suitable substrates to assess the activity of a photo-catalyst.

January, 2020 | DOI: 10.1016/j.arabjc.2017.05.014

Effect of Gold Particles Size over Au/C Catalyst Selectivity in HMF Oxidation Reaction

Megias-Sayago, C; Lolli, A; Bonincontro, D; Penkova, A; Albonetti, S; Cavani, F; Odriozola, JA; Ivanova, S
Chemcatchem (2020)


A series of gold nanoparticles in the 4-40 nm range were prepared, immobilized on activated carbon and further tested, at low base concentration, in the catalytic oxidation of 5-hydroxymethyl furfural (HMF) to 2,5-furandicarboxylic acid (FDCA). Gold particles size variation has no influence on HMF conversion but significantly affects product selectivity and carbon balance. This behavior is ascribed to the thermodynamically favorable oxygen reduction reaction on Au(100) faces. As the gold particle size decreases the Au(100)/Au(111) exposure ratio, estimated by using the van Hardeveld-Hartog model, increases as well as the FDCA selectivity. The smaller the gold particle size the smaller the 5-hydroxymethyl-2-furancarboxylic acid (HMFCA) to FDCA ratio pointing to the gold size dependent behavior of the oxidation of the alcohol function of the HMF molecule.

January, 2020 | DOI: 10.1002/cctc.201901742

Obituary: Prof. José Manuel Criado

Perez-Maqueda, LA; Real, C; Gotor, FJ; Alcala, MD; Malek, J; Koga, N
Journal of Thermal Analysis and Calorimetry, (2020)


Evaluation of Au–ZnO, ZnO/Ag2CO3 and Ag–TiO2 as Photocatalyst for Wastewater Treatment

Murcia, J.J.; Hernández, J.S.;Rojas, H.; Moreno-Cascante, J.; Sánchez-Cid, P.; Hidalgo, M.C.; Navío, J.A.; Jaramillo-Páez, C.
Topics in Catalysis, (2020)


In this work series of photocatalysts based on ZnO modified by Au and Ag2CO3 addition and Ag–TiO2 materials were synthesized and evaluated in the treatment of handicrafts factories wastewater and water samples taken from a highly polluted river. In general, it was found that ZnO series were more effective in the bacteria elimination than the commonly used TiO2 semiconductor. It was also observed that the metal (Au, Ag) or silver carbonate addition significantly increases the photocatalytic activity of ZnO and TiO2. It was determined that the content of the metal or carbonate added is an important factor to take into account in order to obtain suitable efficiency in the photocatalytic process, so, for example in the case of the river water samples the increase of Ag2CO3 content from 1 to 5%, had a detrimental effect over the bacteria elimination. The optimal conditions for dyes photodegradation and bacteria elimination were found by using a response surface study and the Au–ZnO (1%) photocatalyst. From this study it was determined that even after recycling this material leads to obtain a removal percentage of these pollutants over than 94%.

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3D Organic Nanofabrics: Plasma-Assisted Synthesis and Antifreezing Behavior of Superhydrophobic and Lubricant-Infused Slippery Surfaces

Alcaire, M; Lopez-Santos, C; Aparicio, FJ; Sanchez-Valencia, JR; Obrero, JM; Saghi, Z; Rico, VJ; de la Fuente, G; Gonzalez-Elipe, AR; Barranco, A; Borras, A
Langmuir, 35 (2019) 16876-16885


Herein, we present the development of supported organic nanofabrics formed by a conformal polymer-like interconnection of small-molecule organic nanowires and nanotrees. These organic nanostructures are fabricated by a combination of vacuum and plasma-assisted deposition techniques to generate step by step, single-crystalline organic nanowires forming one-dimensional building blocks, organic nanotrees applied as three-dimensional templates, and the polymer-like shell that produces the final fabric. The complete procedure is carried out at low temperatures and is compatible with an ample variety of substrates (polymers, metal, ceramics; either planar or in the form of meshes) yielding flexible and low solid-fraction three-dimensional nanostructures. The systematic investigation of this progressively complex organic nanomaterial delivers key clues relating their wetting, nonwetting, and anti-icing properties with their specific morphology and outer surface composition. Water contact angles higher than 150° are attainable as a function of the nanofabric shell thickness with outstanding freezing-delay times (FDT) longer than 2 h at −5 °C. The role of the extremely low roughness of the shell surface is settled as a critical feature for such an achievement. In addition, the characteristic interconnected microstructure of the nanofabrics is demonstrated as ideal for the fabrication of slippery liquid-infused porous surfaces (SLIPS). We present the straightforward deposition of the nanofabric on laser patterns and the knowledge of how this approach provides SLIPS with FDTs longer than 5 h at −5 °C and 1 h at −15 °C.

December, 2019 | DOI: 10.1021/acs.langmuir.9b03116