Jose J Calvino

Jose J Calvino
Universidad de Cádiz | UCA · Department of Material Science and Metallurgy Engineering and Inorganic Chemistry

PhD

About

348
Publications
36,302
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Introduction
Jose J Calvino currently works at the Department of Material Science and Metallurgy Engineering and Inorganic Chemistry, Universidad de Cádiz. Jose J does research in Chemistry, Electron Microscopy, Catalysis and Materials Chemistry. His current projects focus on the following topics: 1.- Advanced Electron Microscopy in Nanocatalyst Characterisation and Development 2.- Ultrathin, nanostructured, surface phases based on lanthanides for Energy and Environment Protection Technologies

Publications

Publications (348)
Article
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Confronting escalating challenges in energy security and environmental sustainability has intensified interest in renewable sources for fuels and chemicals. Among the most promising alternatives, sugars derived from biomass are emerging as a cornerstone in advancing an environmentally sustainable economy. Within this framework, the development of s...
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The endeavor of sustainable chemistry has led to significant advancements in green methodologies aimed at minimizing environmental impact while maximizing efficiency. Herein, a straightforward synthesis of benzimidazoles by reductive coupling of o‐dinitroarenes with aldehydes is reported for the first time in aqueous media while using a non‐noble m...
Article
A combined surface science/microreactor approach was applied to examine interface effects in ethylene hydrogenation on carbon-supported Ag, Au, and Cu nanoparticle catalysts. Turnover frequencies (TOFs) were substantially higher for supported catalysts than for (unsupported) polycrystalline metal foils, especially for Ag. Spark ablation of the corr...
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A novel PtIn@K‐MFI material has been designed by post‐synthetical incorporation of In to Pt@K‐MFI, resulting in an active and selective alkane dehydrogenation catalyst with improved regenerability relative to the state‐of‐the‐art PtSn@K‐MFI benchmark, and without the requirement of large excess of In and/or harsh activation conditions. image
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Rational design of effective catalyst demands a profound understanding of active-site structures. Single-atom supported powder catalysts, depicting unique features like enhanced metal dispersion, hold promise in different applications. Here, we present an approach to directly quantify the detailed structural nature of metal sites in single-atom, hi...
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Ce and Zr oxides have been tested in the oxidation of cyclohexane to KA oil because of the possibility to tune their crystal structure and redox properties by introducing defects, and of modifying their mechanical and thermal stability. The redox properties of the two oxides, prepared by the inverse microemulsion technique, have been tuned by homog...
Article
This work is devoted to evaluating the relationship between the oxygen content and catalytic activity in the CO oxidation process of the 6H-type BaFeO3−δ system. Strong evidence is provided about the improvement of catalytic performance with increasing Fe average oxidation state, thus suggesting the involvement of lattice oxygen in the catalytic pr...
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At present, transmission electron microscopy is regarded as the main option when dealing with phase characterization for materials at a nanometric scale. The development and improvement of complementary techniques such as energy-dispersive X-ray spectroscopy (EDS), electron energy loss spectroscopy (EELS), imaging detectors and associated computati...
Preprint
This work is devoted to evaluating the relationship between oxygen content and catalytic activity on the CO oxidation process of the 6H-type BaFeO3-δ system, showing that a higher Fe oxidation state improved the catalytic performance of the oxides, confirming the involvement of the lattice oxygen in the catalytic process. The redox behavior of the...
Article
Recently, there has been a growing interest in using MOF templating to synthesize heterogeneous catalysts based on metal nanoparticles on carbonaceous supports. Unlike the common approach of direct pyrolysis of PdIn-MOFs at high temperatures, this work proposes a reductive chemical treatment under mild conditions before pyrolysis (resulting in PdIn...
Preprint
This work is devoted to evaluating the relationship between oxygen content and catalytic activity on the CO oxidation process of the 6H-type BaFeO3-δ system, showing that a higher Fe oxidation state improved the catalytic performance of the oxides, confirming the involvement of the lattice oxygen in the catalytic process. The redox behavior of the...
Article
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Zeolitic materials enriched in phosphorus and nitrogen, with a pronounced content for this last element, were obtained from natural clinoptilolite (CLI) treated with ammonium hydrogenphosphate (DAP) and urea. The interaction of phosphorus and nitrogen species retained on CLI was analyzed using different research methods. FTIR spectra showed the pre...
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MXenes, a family of two-dimensional (2D) transition metal carbides, have been discovered as exciting candidates for various energy storage and conversion applications, including green hydrogen production by water splitting. Today, these materials mostly remain interesting objects for in-depth fundamental studies and scientific curiosity due to issu...
Article
The evolution of the structure and composition of the system of particles in two Ce0.62Zr0.38O2-supported bimetallic catalysts based on Au and a 4d metal (Ru or Pd) under high temperature conditions and different reducing and oxidizing environments has been followed by means of Identical Location Scanning Transmission Electron Microscopy (IL-STEM)....
Article
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Zeolites containing Rh single sites stabilized by phosphorous were prepared through a one-pot synthesis method and are shown to have superior activity and selectivity for ethylene hydroformylation at low temperature (50 °C). Catalytic activity is ascribed to confined Rh2O3 clusters in the zeolite which evolve under reaction conditions into single R...
Article
Accurate 3D nanometrology of catalysts with small nanometer-sized particles of light 3d or 4d metals supported on high-atomic-number oxides is crucial for understanding their functionality. However, performing quantitative 3D electron tomography analysis on systems involving metals like Pd, Ru, or Rh supported on heavy oxides (e.g., CeO2) poses sig...
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The “Gold Dust Defect” that sometimes appears on the surface of the AISI 430 ferritic stainless steel has been related to an improper recrystallization of the material. Hot-rolling, a decisive step in the production process, seems the step where this defect is induced and temperature during this treatment plays a key role. To trace back the origin...
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Sub‐nanometer metal clusters have special physical and chemical properties, significantly different from those of nanoparticles. However, there is a major concern about their thermal stability and susceptibility to oxidation. In situ X‐ray Absorption spectroscopy and Near Ambient Pressure X‐ray Photoelectron spectroscopy results reveal that support...
Article
The combination of structural characterization at atomic resolution, chemical data, and theoretical insights has revealed the unique nanostructures which develop in ceria supported on yttria-stabilized zirconia (YSZ) after being submitted to high-temperature reducing treatments. The results show that just a small ceria loading is needed for creatin...
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Gold-metallic nanofibrils were prepared from three different iso-apoferritin (APO) proteins with different Light/Heavy (L/H) subunit ratios (from 0% up to 100% L-subunits). We show that APO protein fibrils have the ability to in situ nucleate and grow gold nanoparticles (AuNPs) simultaneously assembled on opposite strands of the fibrils, forming hy...
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The present work aims to assess the impact of morphology and reducibility on lanthanum-doped ceria nanocatalysts with controlled morphology on the NO oxidation reaction. Specifically, samples were prepared using a hydrothermal method incorporating lanthanum at varying molar concentrations (0, 5, 10, and 15 mol.%) into ceria with a controlled morpho...
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The generation of methane fuel using surplus renewable energy with CO2 as the carbon source enables both the decarbonization and substitution of fossil fuel feedstocks. However, high temperatures are usually required for the efficient activation of CO2. Here we present a solid catalyst synthesized using a mild, green hydrothermal synthesis that inv...
Article
Few-layer black phosphorus (FLBP), a technologically important 2D material, faces a major hurdle to consumer applications: spontaneous degradation under ambient conditions. Blocking the direct exposure of FLBP to the environment has remained the key strategy to enhance its stability, but this can also limit its utility. In this paper, a more ambiti...
Article
The oxygen stoichiometry of hollandite, KxMnO2-δ, nanorods has been accurately determined from a quantitative analysis of scanning-transmission electron microscopy (STEM) X-Ray Energy Dispersive Spectroscopy (XEDS) experiments carried out in chrono-spectroscopy mode. A methodology combining 3D reconstructions of high-angle annular dark field electr...
Article
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The "gold dust defect" (GDD) appears at the surface of ferritic stainless steels (FSS) and degrades their appearance. Previous research showed that this defect might be related to intergranular corrosion and that the addition of aluminium improves surface quality. However, the nature and origin of this defect are not properly understood yet. In thi...
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Using a nanostructured platform (a controlled‐shape nano‐oxide) and conventional wet impregnation techniques, powder‐type materials have been prepared in which atomically thin surface layers are deposited under very mild conditions. More importantly, an advanced methodology, combining energy dispersive X‐ray spectroscopy‐scanning transmission elect...
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Correction for ‘Photocatalytic removal of benzene over Ti 3 C 2 T x MXene and TiO 2 –MXene composite materials under solar and NIR irradiation’ by Sergii A. Sergiienko et al. , J. Mater. Chem. C , 2022, 10 , 626–639, https://doi.org/10.1039/D1TC03826E.
Article
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Finding simple, easily controlled, and flexible synthetic routes for the preparation of ternary and hybrid nanostructured semiconductors is always highly desirable, especially to fulfill the requirements for mass production to enable application to many fields such as optoelectronics, thermoelectricity, and catalysis. Moreover, understanding the un...
Article
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The aim of this article is to study the catalytic capacities of gold nanoparticles based on a layered double hydroxide prepared by a depo-precipitation method in oxidation. The main interest of this work is to prove the possibility of using these materials as catalysis for selective oxidation for succinic acid production. The textural and morpholog...
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Oxygen mass transport in perovskite oxides is relevant for a variety of energy and information technologies. In oxide thin films, cation nonstoichiometry is often found but its impact on the oxygen transport properties is not well understood. Here, we used oxygen isotope exchange depth profile technique coupled with secondary ion mass spectrometry...
Article
The ability to mimic protein-based oxidase with multi-functional inorganic nanozymes would greatly advance biomedical and clinical practices. Praseodymia (PrOx) nanorods (NRs) and nanoparticles (NPs) have been synthesized using hydrothermal and precipitation methods. Both PrOx catalysts with different morphologies exhibit significantly higher oxida...
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The ''Gold Dust Defect'' affects the surface quality of AISI 430 ferritic stainless steels. However, there is a very limited number of studies focusing on it. To better understand its nature, we have combined several techniques, such as x- ray photoelectron spectroscopy, atomic force microscopy, and transmission electron microscopy, in order to ext...
Article
Full-text available
The aim of this article is to study the catalytic capacities of gold nanoparticles based on a layered double hydroxide prepared by a depo-precipitation method in oxidation. The main interest of this work is to prove the possibility of using these materials as catalysis for selective oxidation for succinic acid production. The textural and morpholog...
Article
Antitumoral Agents In article number 2113028, M. Arturo López‐Quintela, Fernando Domínguez, and co‐workers report that Ag5 clusters show unique catalytic activities to oxidize thiols. They catalyze the complete oxidation of thiols present in cysteine, glutathione, and thioredoxin. This oxidation is tunable by relevant biological oxidants species (h...
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Electron Tomography (ET) reconstructions can be analysed, via segmentation techniques, to obtain quantitative, 3D-information about individual nanoparticles in supported catalysts. This includes values of parameters out of reach for any other technique, like their volume and surface, which are required to determine the dispersion of the supported p...
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Probiotic bacteria were used as carriers of metallic nanoparticles to develop innovative oral agents for hyperthermia cancer therapy. Two synthetic strategies were used to produce the different therapeutic agents. First, the probiotic bacterium Lactobacillus fermentum was simultaneously loaded with magnetic (MNPs) and gold nanoparticles (AuNPs) of...
Article
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Low atomicity clusters present properties dependent on the size, due to the quantum confinement, with well‐defined electronic structures and high stability. Here it is shown that Ag5 clusters catalyze the complete oxidation of sulfur to S⁺⁶. Ag5 catalytic activity increases with different oxidant species in the order O2 ≪ H2O2 < OH•. Selective oxid...
Article
We report an initial magnetic study of highly crystalline nanoparticles of the layered-kagome compound BaCo3(VO4)2(OH)2. Quasi-spherical nanoparticles with size in the range of 9-25 nm were elaborated for the first time via a new synthetic route at ambient pressure. Rietveld refinement of X-ray diffraction data, vibrational spectrocopies and high-r...
Article
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The encapsulation of bioactive natural products has emerged as a relevant tool for modifying the poor physicochemical properties often exhibited by agrochemicals. In this regard, natural guaiane-type sesquiterpene lactones isolated from Cynara cardunculus L. have been encapsulated in a core/shell nanotube@agrochemical system. Monitoring of the F a...
Article
Modern life-style is creating an indoor generation: human beings spend approximately 90% of their time indoors, almost 70% of which is at home – this trend is now exacerbated by the lockdowns/restrictions imposed due to the COVID-19 pandemic. That large amount of time spent indoors may have negative consequences on health and well-being. Indeed, po...
Article
Full-text available
Subnanometric metal species confined inside the microporous channels/cavities of zeolites have been demonstrated as stable and efficient catalysts. The confinement interaction between the metal species and zeolite framework has been proposed to play the key role for stabilization, though the confinement interaction is elusive to be identified and m...
Article
The preferential oxidation of CO in H2-rich mixtures has been studied using Ce0.8Zr0.2O2-supported Cu catalysts containing increasing amounts of copper [1 wt% (Cu1/CZ), 2 wt% (Cu2/CZ) and 4 wt% (Cu4/CZ)]. The oxide support was prepared by co-precipitation and the copper was incorporated using the wetness impregnation method. The catalysts were char...
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We report the structural and chemical investigation of nine presolar silicate grains from the CH3/CB b 3 chondrite Isheyevo and CR2 chondrite Northwest Africa (NWA) 801. Five of these grains belong to group 1, likely condensed in low-to intermediate-mass asymptotic giant branch (AGB) stars, super-AGB stars, or core-collapse supernovae, while the re...
Article
This paper presents new models for segmentation of 2D and 3D Scanning-Transmission Electron Microscope images based on the ordered median function. The main advantage of using this function is its good adaptability to the different types of images to be studied due to the wide range of weight vectors that can be cast. Classical segmentation models...
Article
Supported Ni catalysts (4.5 wt%) using a Ce-Zr oxide (18/82 molar ratio and a ceria-rich surface) depicting advanced redox properties, were deposited by washcoating over cordierite honeycombs (230 and 400 cpsi). FIB-STEM unveiled nanostructure details otherwise undistinguishable by conventional techniques. The catalytic performance was evaluated in...
Article
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Redox properties on CeO 2 /TiO 2 system are reversibly modified with SRMO and SRSO treatments. The single low temperature peak featuring on SRMO samples is coming from a highly dispersed ceria thin layer extended over the TiO 2 surface.
Preprint
Full-text available
Modern life-style is creating an indoor generation: human beings spend approximately 90% of their time indoors, almost 70% of which is at home – this trend is now exacerbated by the lockdowns/restrictions imposed due to the COVID-19 pandemic. That large amount of time spent indoors may have negative consequences on health and well-being. Indeed, po...
Article
Full-text available
MXenes, a family of two-dimensional (2D) transition metal carbides, nitrides and carbonitrides based on earth-abundant constituents, are prospective candidates for energy conversion applications, including photocatalysis. While the activity of individual MXenes towards various photocatalytic processes is still debatable, these materials were proved...
Article
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A family of iron-doped manganese-related hollandites, KxMn1–yFeyO2−δ (0 ≤ y ≤ 0.15), with high performance in CO oxidation have been prepared. Among them, the most active catalyst, K0.11Mn0.876Fe0.123O1.80(OH)0.09, is able to oxidize more than 50% of CO at room temperature. Detailed compositional and structural characterization studies, using a wid...
Article
Magnetic and conducting composites of cobalt ferrite nanoparticles and poly(aniline) have been synthesized in acid media by the oxidative polymerization of aniline in the presence of a dispersion of magnetic nanoparticles, using Fe(III) ions as an oxidizing agent. The materials have been characterized by X-ray diffraction studies, X-ray fluorescenc...
Article
Ceria (CeO2) is a ubiquitous component in catalysts for environmental protection processes, especially those devoted to CO2 valorisation. Aimed at preparing ceria-based nanomaterials with enhanced CO2 adsorption and activation properties, both the surface acid-base and redox features of ceria nanocubes were modulated by a novel, simple, wet chemist...
Article
The texture, structure, composition, and electronic state of new and used monolithic Mn-Cu catalysts were studied. Characterisation was performed at different scales and spatial resolution by combining STEM-FIB and imaging techniques (STEM-HAADF) and spectroscopy (STEM-EDX and EELS of space resolution). A thickness of the alumina layer that varies...