Solid State Processing of BCZT Piezoceramics Using Ultra Low Synthesis and Sintering Temperatures.

Lead-free (BaCa) (Ti Zr) O (BCZT) ceramics were prepared by a solid-state route (SSR) using ultra-low synthesis (700 °C/30 min and 700 °C/2 h) and sintering temperatures (from 1150 °C to 1280 °C), due to prior activation and homogenization by attrition milling of the starting high purity raw materials for 6 h before the synthesis and of the calcined powders for 3 h before the sintering. The comparison of the thermal analysis of the mixture of the starting raw materials and the same mixture after 6 h attrition milling allowed to evidence the mechanisms of activation, resulting in a significant decrease of the perovskite formation temperature (from 854 °C down to 582 °C). The secondary phases that limit the functional properties of the ceramic and their evolution with the sintering conditions were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM), which allowed the design of a two-step sintering method to eliminate them.

Unveiling redox mechanism at the iron centers in the mechanochemically activated conversion of CO in the presence of olivine.

Unlabelled: The transformation of olivine during the conversion of CO to light hydrocarbons activated by mechanochemical treatments at different impact frequencies was studied by a combination of several complementary characterization methods including X-ray diffraction, Raman and Fe Mössbauer spectroscopy. Several olivine samples were studied as a function of the milling time, indicating the gradual transformation of Fe-containing olivine into new Fe-containing weathering products including iron oxides, magnesium iron carbonates and silicates. The results presented here complement those of a previous study on the weathering process of olivine promoted by mechanochemical activation, by demonstrating the role of the redox activity of the iron species during the activation process.

As Uptake from Nanostructured Iron Oxides and Oxyhydroxides: The Complex Interplay between Sorbent Surface Chemistry and Arsenic Equilibria.

Iron oxides/oxyhydroxides, namely maghemite, iron oxide-silica composite, akaganeite, and ferrihydrite, are studied for As and As removal from water in the pH range 2-8. All sorbents were characterized for their structural, morphological, textural, and surface charge properties. The same experimental conditions for the batch tests permitted a direct comparison among the sorbents, particularly between the oxyhydroxides, known to be among the most promising As-removers but hardly compared in the literature.

State-of-the-art biosynthesis of tin oxide nanoparticles by chemical precipitation method towards photocatalytic application.

Tin oxide (SnO) with versatile properties is of substantial standing for practical application, and improved features of the material are demonstrated in the current issue through the integration of nanotechnology with bio-resources leading to what is termed as biosynthesis of SnO nanoparticles (NPs). This review reveals the recent advances in biosynthesis of SnO NPs by chemical precipitation method focused on distinct methodologies, characterization, and reaction mechanism along with a photocatalytic application for dye degradation. According to available literature reviews, numerous bio-based precursors selectively extracted from biological substrates have effectively been applied as capping or reducing agents to achieve the metal oxide NPs.

MgNb O Modified K Na NbO Eco-Piezoceramics: Scalable Processing, Structural Distortion and Complex Impedance at Resonance.

In this work, piezoceramics of the lead-free composition K Na NbO with an increasing amount of MgNb O (0, 0.5, 1, 2 wt.%) were prepared through conventional solid-state synthesis and sintered in air atmosphere at 1100 °C.

Processing Optimization and Toxicological Evaluation of "Lead-Free" Piezoceramics: A KNN-Based Case Study.

Due to the ever-increasing limitations of the use of lead-based materials, the manufacturing of lead-free piezoceramics with competitive piezoelectric properties and established nontoxicity is considered a priority for the scientific and industrial community. In this work, a lead-free system based on sodium potassium niobate (KNN), opportunely modified with MgNbO (MN), was prepared through a combination of a mechanochemical activation method and air sintering, and its toxicity was evaluated. The effect of the mechanical processing on the microstructure refinement of the processed powders was established by X-ray diffraction and the average crystallite size content of the NbO species was evaluated.

Boron Nitride-Titania Mesoporous Film Heterostructures.

The fabrication of optically active heterostructures in the shape of mesostructured thin films is a highly challenging task. It requires an integrated process to allow in one-step incorporating the two-dimensional materials within the mesoporous ordered host without disrupting the pore organization. Hexagonal boron nitride (BN) nanosheets have been successfully introduced into titania mesoporous films using a template-assisted sol-gel synthesis and evaporation-induced self-assembly.

synchrotron radiation investigation of VO-NbO metastable compounds: transformational kinetics at high temperatures with a new structural solution for the orthorhombic VNbO phase.

Due to the considerable interest in vanadium niobium oxides as a lithium storage material, the kinetics and transformation processes of the V2O5-5Nb2O5 system have been investigated by in situ synchrotron powder X-ray diffraction. The diffraction data after the thermal treatments selected with a view on the most significant features were supplemented with specific ex situ experiments conducted using a laboratory rotating anode X-ray diffractometer. The morphological changes of the mixed powders assuming an amorphous and nanocrystalline solid solution structure as a function of the temperature were inspected by scanning electron microscopy observations.

Defect-assisted synthesis of magneto-plasmonic silver-spinel ferrite heterostructures in a flower-like architecture.

Artificial nano-heterostructures (NHs) with controlled morphology, obtained by combining two or more components in several possible architectures, make them suitable for a wide range of applications. Here, we propose an oleate-based solvothermal approach to design silver-spinel ferrite flower-like NHs. Small oleate-coated silver nanoparticles were used as seeds for the growth of magnetic spinel ferrite (cobalt ferrite and spinel iron oxide) nanodomains on their surface.

Boron oxynitride two-colour fluorescent dots and their incorporation in a hybrid organic-inorganic film.

Bottom-up synthesis of fluorescent boron-nitride based dots is a challenging task because an accurate design of the structure-properties relationship is, in general, difficult to achieve. Incorporation of the dots into a solid-state matrix is also another important target to develop light-emitting devices. Two-colour fluorescent boron oxynitride nanodots have been obtained by a bottom-up synthesis route and incorporated into a hybrid organic-inorganic film.

A mechanochemical route for the synthesis of VNbO and its structural re-investigation using structure solution from powder diffraction data.

A new and solvent-free synthesis route has been adopted and optimized to prepare crystalline VNbO from the mechanochemical reaction between NbO and VO as starting reagents. The substantially amorphous mixture of equimolar pentoxide V and Nb metals observed after extended mechanical treatment transforms into a crystalline powder following calcination under mild conditions at 710 K. The structure solution of the X-ray diffraction pattern using a global optimization approach, combined with Rietveld refinement, points to a space group P222 (no.

Remarkable hydrogen storage properties of MgH doped with VNbO.

The present work concerns the catalytic effect of VNbO, a ternary oxide prepared via a solid-state route, on the sorption performance of MgH. Three doped systems, namely 5, 10 and 15 wt% VNbO-MgH have been prepared by ball milling and thoroughly characterized. Hydrogen sorption, evaluated by temperature programmed desorption experiments, revealed a significant reduction of the desorption temperature from 330 °C for the un-doped sample (prepared and tested for comparison) to 235 °C for the VNbO-doped sample.

Structural and kinetic investigation of the hydride composite Ca(BH4)2 + MgH2 system doped with NbF5 for solid-state hydrogen storage.

Designing safe, compact and high capacity hydrogen storage systems is the key step towards introducing a pollutant free hydrogen technology into a broad field of applications. Due to the chemical bonds of hydrogen-metal atoms, metal hydrides provide high energy density in safe hydrogen storage media. Reactive hydride composites (RHCs) are a promising class of high capacity solid state hydrogen storage systems.

Tuning the phase transition of ZnO thin films through lithography: an integrated bottom-up and top-down processing.

An innovative approach towards the physico-chemical tailoring of zinc oxide thin films is reported. The films have been deposited by liquid phase using the sol-gel method and then exposed to hard X-rays, provided by a synchrotron storage ring, for lithography. The use of surfactant and chelating agents in the sol allows easy-to-pattern films made by an organic-inorganic matrix to be deposited.

Mesoporous Titania Powders: The Role of Precursors, Ligand Addition and Calcination Rate on Their Morphology, Crystalline Structure and Photocatalytic Activity.

We evaluate the influence of the use of different titania precursors, calcination rate, and ligand addition on the morphology, texture and phase content of synthesized mesoporous titania samples, parameters which, in turn, can play a key role in titania photocatalytic performances. The powders, obtained through the evaporation-induced self-assembly method, are characterized by means of X-Ray Powder Diffraction (XRPD) measurements, N₂ physisorption isotherms and transmission electron microscopy. The precursors are selected basing on two different approaches: the acid-base pair, using TiCl₄ and Ti(OBu)₄, and a more classic route with Ti(OPr)₄ and HCl.

Magnesium imide: synthesis and structure determination of an unconventional alkaline earth imide from decomposition of magnesium amide.

Magnesium imide (MgNH) was produced by monitoring the decomposition process of magnesium amide with in situ neutron diffraction. Significant changes in the structure of magnesium amide are detected during heat treatment and eventually result in the formation of crystalline MgNH. A model for the crystal structure of magnesium imide (MgNH) is presented for the first time.

Cremation practices coexisting at the S'Illot des Porros Necropolis during the Second Iron Age in the Balearic Islands (Spain).

The necropolis of S'Illot des Porros, one of the most important prehistoric funerary sites of the Balearic Islands (Spain), was in use from the VIth and Vth century BCE until the Ist century CE. Located in a funerary area which contains two cementeries and one sanctuary, this site is constituted by three funerary chambers named A, B and C, respectively. Investigations on all the human burnt bone remains of the chambers, carried out mainly by the X-ray diffraction and supplemented in some cases by Fourier Transform Infrared spectroscopy pointed to the simultaneous use of inhumation and cremation funerary rites, probably due to existing social differences.

Study of sorption processes and FT-IR analysis of arsenate sorbed onto red muds (a bauxite ore processing waste).

In this study we evaluated the arsenate adsorption capacity of red muds (RM), wastes tailing from the alumina production, at different pH values (4, 7, and 10). RM samples were artificially enriched in batch tests with solutions containing increasing concentrations of As(V). The pH of the solution significantly affected the adsorption, which increased with the decrease of pH.

The potential of X-ray diffraction in the analysis of burned remains from forensic contexts.

In view of the difficulties in extracting quantitative information from burned bone, we suggest a new and accurate method of determining the temperature and duration of burning of human remains in forensic contexts. Application of the powder X-ray diffraction approach to a sample of human bone and teeth allowed their microstructural behavior, as a function of temperature (200-1000 degrees C) and duration of burning (0, 18, 36, and 60 min), to be predicted. The experimental results from the 57 human bone sections and 12 molar teeth determined that the growth of hydroxylapatite crystallites is a direct and predictable function of the applied temperature, which follows a nonlinear logistic relationship.

Sorption processes and XRD analysis of a natural zeolite exchanged with Pb(2+), Cd(2+) and Zn(2+) cations.

In this study the Pb(2+), Cd(2+) and Zn(2+) adsorption capacity of a natural zeolite was evaluated in batch tests at a constant pH of 5.5 by polluting this mineral with solutions containing increasing concentrations of the three cations to obtain adsorption isotherms. In addition X-ray powder diffraction (XRD) was used to investigate the changes of zeolite structure caused by the exchange with cations of different ionic radius.