A non-hydrolytic sol-gel approach for the preparation of MgxAl2(1-x)Ti(1+x)O5 powders

The study of non-hydrolytic reactions for the synthesis of MgxAl2(1-x)Ti(1+x)O5 solid solution with x = 0.6 is reported. The reagents chosen were Al(OsBu)(3), Ti(OiPr)(4), TiCl4 and Mg(NO3)(2).6H(2)O in toluene. The reactions were followed using C-13 Nuclear Magnetic Resonance (NMR) spectroscopy. Sol-gel synthesized powders were calcined in air at 300, 500, 1000, and 1200degreesC for 1 h. The powders were analysed by X-Ray Diffraction (XRD) demonstrating the formation of a Mg0.6Al0.8Ti1.6O5 phase in samples treated at the higher calcination temperature

A covalent organic/inorganic hybrid proton exchange polymeric membrane: synthesis and characterization

Commercial polyetheretherketone (Victrex PEEK) was sulfonated up to 90% degree of sulfonation (DS), then reacted with SiCl4 to obtain a hybrid polymer. The product was characterized by 29-Si NMR and ATR/FTIR spectroscopies demonstrating the formation of covalent bonds between the organic and inorganic components. No dispersed inorganic silicon was present in the product as evidenced by the lack of any resonance at 100 ppm. Despite the high DS the physicochemical properties of the hybrid were suitable for the preparation of membranes exhibiting high and stable conductivity values (10K2 S/cm), hence suitable for application as ion exchange membrane

Sulfonated polyether ether ketone-based composite membranes doped with a tungsten-based inorganic proton conductor for fuel cell applications

Sulfonated polyether ether ketone (SPEEK)-based composite membranes doped with hydrated tungsten oxide were prepared and studied for proton exchange membrane applications. Hydrated tungsten oxide (W O3 ·2 H2 O) was synthesized via acidic hydrolysis of sodium tungstate and its structure and physicochemical features were investigated by thermogravimetric analysis (TG), X-ray diffraction (XRD), and electrochemical impedance spectroscopy (EIS). SPEEK/ W O3 ·2 H2 O composite membranes were prepared by mixing proper amounts of SPEEK and hydrated W O3 in dimethylacetamide as casting solvent. The composite membranes were characterized by XRD, TG-DTA, EIS, and water uptake measurements as a function of the oxide content in the membrane. In particular, XRD patterns as well as TG measurements indicated the existence of a coordinative interaction between the water molecules of tungsten oxide and the SPEEK sulfonic acid groups. This interaction lead to the enhancement of the membrane proton conductivity, as well as of their properties, from the point of view of heat resistance and water solubility. In fact, the addition of tungsten oxide resulted in higher proton conductivity, improved heat resistance, and lower water solubility. © 2006 The Electrochemical Society. All rights reserved

Thick-film gas sensors based on vanadium-titanium oxide powders prepared by sol-gel synthesis

Two titania powders modified by 10 at.% of vanadium were prepared by two different sol-gel routes. The powders fired at 650 °C had the rutile structure. These powders were used to produce prototype thick-film sensors. Four series of thick-film samples were fabricated by screen-printing, fired for 1 h at 650 and 850 °C. The morphology and gas-sensing properties were examined and compared with those of pure and Ta-added titania films, previously studied by the authors. Ta addition inhibited the anatase-to-rutile phase transformation during heating and was also effective in keeping the TiO2 grain size in the nanometre range. On the contrary, V addition facilitated the anatase-to-rutile phase transformation. Thick films obtained from the two powders had similar conductance behaviour vs. temperature. The gas response of the films was affected by both the grain size and firing temperature. © 2003 Elsevier Ltd. All rights reserved

High Differentiation among Eight Villages in a Secluded Area of Sardinia Revealed by Genome-Wide High Density SNPs Analysis

To better design association studies for complex traits in isolated populations it's important to understand how history and isolation moulded the genetic features of different communities. Population isolates should not “a priori” be considered homogeneous, even if the communities are not distant and part of a small region. We studied a particular area of Sardinia called Ogliastra, characterized by the presence of several distinct villages that display different history, immigration events and population size. Cultural and geographic isolation characterized the history of these communities. We determined LD parameters in 8 villages and defined population structure through high density SNPs (about 360 K) on 360 unrelated people (45 selected samples from each village). These isolates showed differences in LD values and LD map length. Five of these villages show high LD values probably due to their reduced population size and extreme isolation. High genetic differentiation among villages was detected. Moreover population structure analysis revealed a high correlation between genetic and geographic distances. Our study indicates that history, geography and biodemography have influenced the genetic features of Ogliastra communities producing differences in LD and population structure. All these data demonstrate that we can consider each village an isolate with specific characteristics. We suggest that, in order to optimize the study design of complex traits, a thorough characterization of genetic features is useful to identify the presence of sub-populations and stratification within genetic isolates

Solid-state synthesis of NASICON (Na3Zr2Si2PO12) using nanoparticle precursors for optimisation of ionic conductivity

In this work, the effect of varying the size of the precursor raw materials SiO2 and ZrO2 in the solid-state synthesis of NASICON in the form Na3Zr2Si2PO12 was studied. Nanoscale and macro-scale precursor materials were selected for comparison purposes, and a range of sintering times were examined (10, 24 and 40 h) at a temperature of 1230 °C. Na3Zr2Si2PO12 pellets produced from nanopowder precursors were found to produce substantially higher ionic conductivities, with improved morphology and higher density than those produced from larger micron-scaled precursors. The nanoparticle precursors were shown to give a maximum ionic conductivity of 1.16 × 10−3 S cm−1 when sintered at 1230 °C for 40 h, in the higher range of published solid-state Na3Zr2Si2PO12 conductivities. The macro-precursors gave lower ionic conductivity of 0.62 × 10−3 S cm−1 under the same processing conditions. Most current authors do not quote or consider the precursor particle size for solid-state synthesis of Na3Zr2Si2PO12. This study shows the importance of precursor powder particle size in the microstructure and performance of Na3Zr2Si2PO12 during solid-state synthesis and offers a route to improved predictability and consistency of the manufacturing process