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A structural and spectroscopic characterization of crystalline rods of Ce0.4Zr0.6O2 grown by the laser floating zone (LFZ) method is presented. A precursor rod of Ce0.4Zr0.6O2 composition was sintered at 1500 ºC in air atmosphere and then processed by the LFZ technique with a CO2 laser. The processed material was characterized by XRD, SEM and Raman spectroscopy. In the as-grown, dark-color processed rod, the Raman spectrum evolves radially from a t’-like one, corresponding to Ce0.37Zr0.63O2 composition, at the edge of the rod, to a very broad and weak, cubic-like one, at the center. The degree of cerium reduction and oxygen non-stoichiometry were determined through measurements of the electronic Raman spectrum of Ce3+. A strong Ce3+ signal was found at the core of the rod, indicating strong reduction, whereas no Ce3+ signal was detected at the edge. To restore oxygen and Ce4+ content a section of the fiber was reoxidized at 620 ºC for 24 h. A very homogeneous spectrum was found in the reoxidized sample, that was assigned to a t’-phase of composition Ce0.42Zr0.58O2.Presentamos una caracterización estructural y espectroscópica de fibras cristalinas de Ce0.4Zr0.6O2 crecidas mediante fusión zonal asistida por láser (LFZ). Una barra del material precursor, de composición Ce0.4Zr0.6O2, fue sinterizada a 1500 ºC en atmósfera de aire y después procesada por LFZ con un láser de CO2. El material procesado fue caracterizado por difracción de rayos X, microscopía electrónica de barrido y espectroscopía Raman. En la fibra recién procesada, de color gris oscuro, el espectro Raman varía radialmente desde un espectro de tipo t’, correspondiente a una composición Ce0.37Zr0.63O2, en el borde de la fibra, hasta un espectro muy ensanchado y débil, de aspecto cúbico, en el centro. El grado de reducción del cerio y la no estequiometría del oxígeno se determinaron a través de las medidas del Raman electrónico del Ce3+. La señal de Ce3+ era muy intensa en el centro de la fibra, lo que indica una fuerte reducción, mientras que no se detectó en el borde. Para restablecer el contenido de oxígeno y de Ce4+ una parte de la fibra fue reoxidada a 620 ºC durante 24 h. El espectro de la muestra reoxidada, de color amarillo pálido y muy homogénea, fue asignado a una fase t’ de composición Ce0.42Zr0.58O2.

Powder of MgFe2O4, previously prepared by solid state reaction, was mechanochemically treated in a centrifugal ball mill in air atmosphere. Different milling conditions has been employed varying ball/powder mass ratio. After low milling time a strong reduction on crystallite size has been detected while the strain lattice increase slowly. The presence of α-Fe2O3 was also observed at different milling time, depending on milling conditions, by means of X-Ray diffraction experiments. Magnetic transition temperatures were evaluated using a thermogravimetric analyser, equipped with a small permanent magnet. An attempt of dependence of magnetic properties with crystallite size has been established.La ferrita MgFe2O4, en forma de polvo y previamente preparada por reacción en estado sólido, se ha sometido a un proceso de molienda mecánica en atmósfera de aire usando un molino centrífugo. Se emplearon diferentes condiciones de molienda variando la relación de peso bolas/ferrita. La variación del tamaño de dominio cristalino o de cristalita y lamicrodeformaciones de red a escala de celda unidad se evaluaron mediante difracción de rayos-X de polvo. Para bajos tiempos de molienda se observó una acusada disminución del tamaño de dominio cristalino, mientras que las microdeformaciones de la red experimentaron un ligero aumento. Así mismo, a partir de determinados tiempos de molienda, se detectó la presencia de α-Fe2O3. Las temperaturas de transición magnética fueron evaluadas a partir de un analizador termogravimétrico equipado con un pequeño imán permanente y se estableció un correlación entre la temperatura de Curie y el tamaño de dominio cristalino.

Given the relevance of lithium and post-lithium batteries as electrochemical energy storage systems, the peculiar crystalline structure of V2O5 and its doping capacity play key roles in lithium-ion battery technology. To integrate them in high-efficiency modules, systematic methodologies are required to estimate the state of charge in a reliable way and predict the Li-V2O5 battery’s performance according to their electrochemical phenomena, including two plateaus in the galvanostatic cycling curves and the dynamic behavior governed by the energy demand. Most state of charge estimation and battery modeling procedures are focused on conventional Li-batteries that show a unique plateau. In this work, we propose a systematic methodology based on the galvanostatic intermittent titration technique and electrochemical impedance spectroscopy to study battery performance in the time and frequency domains, respectively. The proposed methodology, with a time–frequency correlation, promotes a deeper understanding of the electrochemical phenomena and general behavior of Li-V2O5 batteries, allowing for its subsequent extrapolation to more complex and higher-capacity lithium and post-lithium batteries used in high-power applications with a minimum error.

Given the relevance of lithium and post-lithium batteries as electrochemical energy storage systems, the peculiar crystalline structure of V2O5 and its doping capacity play key roles in lithium-ion battery technology. To integrate them in high-efficiency modules, systematic methodologies are required to estimate the state of charge in a reliable way and predict the Li-V2O5 battery's performance according to their electrochemical phenomena, including two plateaus in the galvanostatic cycling curves and the dynamic behavior governed by the energy demand. Most state of charge estimation and battery modeling procedures are focused on conventional Li-batteries that show a unique plateau. In this work, we propose a systematic methodology based on the galvanostatic intermittent titration technique and electrochemical impedance spectroscopy to study battery performance in the time and frequency domains, respectively. The proposed methodology, with a time–frequency correlation, promotes a deeper understanding of the electrochemical phenomena and general behavior of Li-V2O5 batteries, allowing for its subsequent extrapolation to more complex and higher-capacity lithium and post-lithium batteries used in high-power applications with a minimum error. [ABSTRACT FROM AUTHOR]

Proton exchange membrane fuel cells (PEMFCs) are an attractive green technology for energy generation. The poor stability and performances under working conditions of the current electrolytes are their major drawbacks. Metal-Organic Frameworks (MOFs) have recently emerged as an alternative to overcome these issues. Here, we propose a robust Zr-phosphonate MOF (UPG-1) bearing labile protons able to act a priori as an efficient electrolyte in PEMFCs. Further, in an attempt to further enhance the stability and conductivity of UPG-1, a proton carrier (the amino acid Lysine, Lys) was successfully encapsulated within its porosity. The behaviors of both solids as an electrolyte were investigated by a complete experimental (impedance spectroscopy, water sorption) and computational approach (MonteCarlo, water sorption). Compared with the pristine UPG-1, the newly prepared Lys@UPG-1 composite showed similar proton conductivity but a higher stability, which allows a better cyclability. This improved cyclability is mainly related to the different hydrophobic-hydrophilic balance of the Lys@UPG-1 and UPG-1 and the steric protection of the reactive sites of the MOF by the Lys.