84 research outputs found
Improving Wood Resistance to Decay by Nanostructured ZnO-Based Treatments
In this study, the maple wood surface was coated with nanostructured zinc oxide, grown on the surface by using a hydrothermal process, and furtherly treated with shellac varnish. Samples obtained both after ZnO treatment and after the final varnish application were characterized by different techniques, i.e., X-ray diffraction (XRD), scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDS), micro-FTIR with attenuated total reflectance (μ-ATR-FTIR), chromatic variation measurements, and contact angle determinations. Analytical results showed that the wood surface was covered by quite a homogeneous array of inorganic nanoparticles and that the natural resin forms a regular film over the ZnO nanostructures. An accelerated aging test was used to evaluate the protecting effectiveness of the treatments towards UV-induced decay of wood material. After the test, wood treated with ZnO and with the shellac/ZnO combination underwent a considerably lower chromatic change if compared to the untreated wood, suggesting an enhanced resistance of the treated maple to the decay due to light exposition. The presence of nanostructured ZnO protects from decay not only the wood substrate but also the shellac film. A microbiology test showed that growth of fungal species, e.g., common mold, is prevented on the wood surface treated with ZnO or with shellac/ZnO, indicating that the nanostructured zinc oxide also provides an effective protection from biodeterioration. The coating obtained by consecutive application of nanosized ZnO particles and shellac varnish combines the excellent aesthetical features and water repellence of the traditional finish with the protecting effectiveness of the nanostructured inorganic component
New materials for Li-ion batteries : synthesis and spectroscopic characterization of Li2(FeMnCo) SiO4 cathode materials
Improving cathode materials is mandatory for next-generation Li-ion batteries. Exploring polyanion compounds with high theoretical capacity such as the lithium metal orthosilicates, Li2MSiO4 is of great importance. In particular, mixed silicates represent an advancement with practical applications. Here we present results on a rapid solid state synthesis of mixed Li2(FeMnCo)SiO4 samples in a wide compositional range. The solid solution in the P21/n space group was found to be stable for high iron concentration or for a cobalt content up to about 0.3 atom per formula unit. Other compositions led to a mixture of polymorphs, namely Pmn21 and Pbn21. All the samples contained a variable amount of Fe3+ ions that was quantified by Mössbauer spectroscopy and confirmed by the TN values of the paramagnetic to antiferromagnetic transition. Preliminary characterization by cyclic voltammetry revealed the effect of Fe3+ on the electrochemical response. Further work is required to determine the impact of these electrode materials on lithium batteries
Structural, spectroscopic and magnetic investigation of the LiFe1-xMnxPO4 (x = 0 - 0.18) solid solution
Different solid state and sol-gel preparations of undoped and Mn substituted cathode material LiFePO4 are investigated. Li3PO4, Fe2P2O7 and Li4P2O7 are detected and quantified by XRPD only in solid state synthesis. In addition, micro-Raman spectra reveal low amount of different iron oxides clusters. EPR data, combined with the results of magnetization measurements, evidence signals from Fe3+ ions in maghemite nanoclusters, and in Li3Fe2(PO4)3. The sol–gel synthesis, showing the lowest amount of impurity phases, seems the most suitable to obtain a promising cathode material. The structural refinement gives new insights into the cation distribution of the Mn doped triphylite structure: (i) about 85% of Mn2+ ions substitutes Fe2+, the remaining 15% being located on the Li site, thus suggesting a structural disorder also confirmed by EPR and micro-Raman results; (ii) Mn ions on the Li site are responsible for the observed slight cell volume expansion
Combined Layer-by-Layer/Hydrothermal Synthesis of Fe3O4@MIL-100(Fe) for Ofloxacin Adsorption from Environmental Waters
: A simple not solvent and time consuming Fe3O4@MIL-100(Fe), synthesized in the presence of a small amount of magnetite (Fe3O4) nanoparticles (27.3 wt%), is here presented and discussed. Layer-by-layer alone (20 shell), and combined layer-by-layer (5 shell)/reflux or /hydrothermal synthetic procedures were compared. The last approach (Fe3O4@MIL-100_H sample) is suitable (i) to obtain rounded-shaped nanoparticles (200-400 nm diameter) of magnetite core and MIL-100(Fe) shell; (ii) to reduce the solvent and time consumption (the layer-by-layer procedure is applied only 5 times); (iii) to give the highest MIL-100(Fe) amount in the composite (72.7 vs. 18.5 wt% in the layer-by-layer alone); (iv) to obtain a high surface area of 3546 m2 g-1. The MIL-100(Fe) sample was also synthesized and both materials were tested for the absorption of Ofloxacin antibiotic (OFL). Langmuir model well describes OFL adsorption on Fe3O4@MIL-100_H, indicating an even higher adsorption capacity (218 ± 7 mg g-1) with respect to MIL-100 (123 ± 5 mg g-1). Chemisorption regulates the kinetic process on both the composite materials. Fe3O4@MIL-100_H performance was then verified for OFL removal at µg per liter in tap and river waters, and compared with MIL-100. Its relevant and higher adsorption efficiency and the magnetic behavior make it an excellent candidate for environmental depollution
Cr and Ni doping of Li4Ti5O12: cation distribution and functional properties
Cr- and Ni-doped Li4Ti5O12 compound has been characterized through the combined use of X-ray powder diffraction, electron paramagnetic resonance (EPR), 7Li nuclear magnetic resonance magic-angle spinning (NMR-MAS), micro-Raman, and magnetization measurements. The doping, occurring on the octahedral site of the cubic Li4Ti5O12 spinel lattice, strongly affects both the local and the average structural properties. The glassy character of the observed EPR signals suggests structural disorder in the stable Li4Ti5O12 matrix and the presence of clustering phenomena or nonhomogeneous distribution of the dopant ion, as also supported by 7Li NMR-MAS, micro-Raman, and magnetization results. The computation by numerical method of the complex EPR signal of the Cr-doped sample suggests that both CrTi and CrLi substitutions occur, giving rise to two distinct EPR components, corresponding to opposite axial distortion of the relative octahedral environments. On the basis of the compositional data, defect models involving oxygen or cation vacancies are proposed to explain the conductivity of the doped material
Pair distribution function analysis and Mössbauer study of defects in microwave-hydrothermal LiFePO 4
Olivine-type LiFePO 4 is nowadays one of the most important cathode materials of choice for high-energy lithium ion batteries. Its intrinsic defectivity, and chiefly the so-called lithium iron anti-site, is one of the most critical issues when envisaging electrochemical applications. This paper reports a combined diffractometric (Synchrotron Radiation XRD with Rietveld and PDF analyses) and spectroscopic (Mössbauer) approach able to give a thorough characterization of the material defectivity. Such analytical procedure has been applied to a sample prepared following an innovative microwave-assisted hydrothermal synthesis route that, in a few minutes, allowed us to obtain a well crystallized material. PDF analysis, which is applied for the first time to this type of battery material, reveals the presence of disorder possibly due to Li/Fe exchange or to a local symmetry lowering. A 5% amount of iron on the lithium site has been detected both by PDF as well as by Mössbauer spectroscopy, which revealed a small percentage of Fe 3+ on the regular sites. © 2012 The Royal Society of Chemistry
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