Preparation of SnO2 whiskers via the decomposition of tin oxalate

A new method for preparing SnO₂ whiskers by the decomposition of SnC₂O₄ is suggested. A Whisker-like morphology of a SnC₂O₄ precipitate was attained via the gradual addition of an oxalic acid solution to a hot SnCl₂ aqueous solution (T > 50^∘C). In comparison, when the solution temperature was either lower than 50^∘C or when ethanol was used as the solvent, the SnC₂O₄ precipitate showed an angular and relatively isotropic morphology. The morphology of the SnC₂O₄ precipitate remained even after its thermal decomposition into SnO₂ at 400^∘C indicating that SnC₂O₄ precipitation is a key step in preparing the whiskers. The formation mechanism of SnO₂ whiskers was explained by the supersaturation during the precipitation of SnC₂O₄.     

Hydration Kinetics and Phase Stability of Dicalcium Silicate Synthesized by the Pechini Process

Reactive dicalcium silicate (Ca₂SiO₄) has been synthesized by the Pechini process, and hydration kinetics studied. With increasing calcination temperature, the amorphous product first crystallizes to α'_L-phase and subsequently to the ß- and γ-phases. The specific surface area, ranging from 40 to 1 m²/g, strongly depends on the calcination temperature of 700°-1200°C for 1 h. Samples with a high surface area have a high water demand; a water/cement ratio >2.0 is required to produce formable pastes in some instances. Hydration kinetics are determined by XRD, ²⁹Si magic-angle spinning nuclear magnetic resonance (MAS NMR), and differential scanning calorimetry/thermogravimetry (DSG/TG). The hydration rate depends only on the surface area, not on the polymorph. Complete hydration occurs in as early as 7 d. Very little calcium hydroxide (Ca(OH)₂) is formed in the most reactive specimens (calcined at 700° and 800°C), which indicates the Ca/Si ratio in C-S-H gels is ∼2.0, but more Ca(OH)₂ forms from samples calcined at higher temperature. The silicate structure of the hydrated Ca₂SiO₄ pastes is investigated using ²⁹Si MAS NMR spectroscopy and trimethylsilylation analysis.     

Calcium Phosphate Bioceramics with Various Porosities and Dissolution Rates

Porous bioceramics, such as hydroxyapatite (HA), tricalcium phosphate (TCP), and biphasic HA/TCP, were fabricated using the polyurethane sponge technique. The porosity of the ceramics was controlled by a multiple coating of the porous body. When a porous body was produced by a single coating, the porosity was ∼90%, and the pores were completely interconnected. When the sintered body was coated five times after the porous network had been made, the porosity decreased to 65%. As the porosity decreased, the strength increased exponentially. The TCP exhibited the highest dissolution rate in a Ringer's solution, and the HA had the lowest rate. The biphasic HA/TCP showed an intermediate dissolution rate.     

Apatite Induction on Ca-Containing Titania Formed by Micro-Arc Oxidation

Ca-containing, particularly CaTiO₃, titania films were prepared by micro-arc oxidation (MAO) of Ti in an electrolytic solution containing calcium acetate monohydrate (CA), and their apatite-inducing ability was evaluated in a simulated body fluid (SBF). The phase, Ca content, and morphology of the films were found to be strongly dependent on the applied voltage. The CaTiO₃-embedded titania was obtained at higher voltages (>300 V). When immersed in SBF, no apatite was induced in all the MAO specimens irrespective of the presence of CaTiO₃, which has been claimed to be an apatite inducer. However, after a hydrothermal treatment at 250°C, apatite was formed on the surfaces of the CaTiO₃-embedded titania after 28 days, which was closely related to the formation of amorphous Ca(OH)₂ and presumably surface Ti–OH groups.     

Chemistry of SiNx thin film deposited by plasma-enhanced atomic layer deposition using di-isopropylaminosilane (DIPAS) and N2 plasma

Silicon nitride (Si₃N₄) films have received great attention not only as dielectric materials for the gate dielectric of transistors and the insulator of capacitors, but also as a buffer layer and etch-stop layer for the semiconductor industry. As the applications of Si₃N₄ film increase, the necessity of investigating a novel deposition process applicable at low temperature has emerged. In this regard, the plasma-enhanced atomic layer deposition (PEALD) technique is attractive as a promising process; however, the Si₃N₄ film deposition process at growth temperatures less than 150?°C using PEALD has not been investigated. In this work, the growth behavior and chemistry of SiN_x (x?<?1.33) film deposited by the PEALD process at various growth temperatures were developed. Insufficient thermal energy from low growth temperature induces an unstable chemical state of deposited film due to the remaining unreacted ligand of adsorbed precursors. This state results in a further chemical reaction to SiO₂ formation by air exposure. Other chemical effects depending on chemical composition and electrical property were also examined in detail.     

Effects of sintering conditions on the microstructure and mechanical properties of SiC prepared using powders recovered from kerf loss sludge

The effects of sintering conditions on the microstructure and mechanical properties of the sintered SiC prepared using the SiC powder recovered from the kerf loss sludge were investigated. The recovered SiC powders were consolidated by spark plasma sintering (SPS) and conventional sintering methods. The effects of sintering temperature, time and methods (SPS and conventional sintering) on the phase, grain size and density of SiC were systematically studied. The Vickers hardness of spark plasma-sintered (SPSed) samples was higher than that of conventional sintered samples due to small grain size. When holding time was increased from 10 to 30 min, the grain size and relative density of SPSed samples were also increased, which lead to the almost constant Vickers hardness by competing effects of grain size and relative density. When holding time was over 30 min, no appreciable change of the relative density and grain size were observed, which can lead to similar values of Vickers hardness. SPS process can be used to make SiC with high density and hardness at relatively low temperature compared with the conventional sintering process.     

New Insight into Microstructure Engineering of Ni-Rich Layered Oxide Cathode for High Performance Lithium Ion Batteries

Ni-rich layered LiNi_xCo_yMn_1−x−yO₂ (LNCM) with Ni content over >90% is considered as a promising lithium ion battery (LIB) cathode, attributed by its low cost and high practical capacity. However, Ni-rich LNCM inevitably suffers rapid capacity fading at a high state of charge due to the mechanochemical breakdown; in particular, the microcrack formation has been regarded as one of the main culprits for Ni-rich layered cathode failure. To address these issues, Ni-rich layered cathodes with a textured microstructure are developed by phosphorous and boron doping. Attributed by the textured morphology, both phosphorous- and boron-doped cathodes suppress microcrack formation and show enhanced cycle stability compared to the undoped cathode. However, there exists a meaningful capacity retention difference between the doped cathodes. By adapting the various analysis techniques, it is shown that the boron-doped Ni-rich layered cathode displays better cycle stability not only by its ability to suppress microcracks during cycling but also by its primary particle morphology that is reluctant to oxygen evolution. The present work reveals that not only restraint of particle cracks but also suppression of oxygen release by developing the oxygen stable facets is important for further improvements in state-of-the-art Li ion battery Ni-rich layered cathode materials.     

Electric and Dielectric Properties of Nb-Doped CaCu3Ti4O12 Ceramics

Pure and Nb-substituted CaCu₃Ti_{4− x} Nb _x O_{12+ x /2} (CCTO, x =0, 0.02, 0.1, 0.2, 0.4) ceramics were prepared by a conventional solid-state sintering, and their electric and dielectric properties were investigated using an impedance analyzer. A single-phase CCTO was obtained up to x =0.2 Nb substitution and the lattice parameter increased with Nb substitution concentration. While the grain size decreased with Nb substitution, the resistivity of the grain boundary decreased. The dielectric constant increased with Nb substitution, and the highest value of ∼420 000 was observed in the x =0.2 Nb-substituted specimen at 10 kHz. The obtained electric and dielectric properties in Nb-substituted CCTO were discussed in terms of the internal barrier layer capacitor model, particularly focusing on a ratio of thickness of the grain boundary region to grain size.     

Uniform Coating of Nanometer-Scale BaTiO3 Layer on Spherical Ni Particles via Hydrothermal Conversion of Ti-Hydroxide

A uniform BaTiO₃ nano layer was coated on spherical Ni particles for multilayer ceramic capacitor applications via a Ti-hydroxide coating using the controlled hydrolysis of a TiCl₄ butanol solution containing (C₂H₅)₂NH (diethylamine, DEA) and its subsequent hydrothermal reaction at various [Ba(OH)₂], residual [DEA], and hydrothermal temperatures. The hydrothermal conversion was successful at [Ba(OH)₂]≥0.065 M (Ba/Ti≥1.3) and T ≥150°C, and the residual DEA in the Ti-hydroxide coating layer not only affected the formation of the BaTiO₃ phase but also resulted in a rough surface morphology. When a minimal amount of DEA was involved in the formation of Ti-hydroxide, a uniform BaTiO₃ coating with a clean surface morphology could be attained, which was confirmed by elemental mapping of the coated powder and the observation of hollow spheres after removing the Ni core. The BaTiO₃ coating was very effective not only in preventing Ni oxidation but also in shifting the starting point of Ni densification to a higher temperature.     

CO gas sensing properties in Pd-added ZnO sensors

Unadded and 0.5 mol% Pd-added ZnO bulk and thin films were prepared by sintering and sputtering, respectively, and their CO gas sensing properties were investigated. The effects of Pd addition, sensing temperature (100–500 °C), and humidity on the CO gas response were discussed. In the bulk sensors, Pd-addition lowered the temperature for the maximum CO gas response (sensitivity) from 400 to 300 °C, whereas the thin film sensors (unadded and Pd-added) exhibited maximum gas response at 200 °C. The Pd-addition enhanced the CO gas response in thin film sensors, and it was also effective for reducing the interference from humidity in both bulk and thin film sensors.