Mechanochemical synthesis of nanoparticulate ZnO–ZnWO4 powders and their photocatalytic activity

In this study, mechanochemical reaction systems with H₂WO₄ as a precursor were investigated for the synthesis of nanoparticulate powders of WO₃, ZnWO₄, and dual-phase (ZnWO₄)_x(ZnO)_1–x. The objective was to establish whether mechanochemical processing can be used to manufacture high activity photocatalysts in the ZnO–WO₃ system. Milling and heat treatment of H₂WO₄ + 12NaCl was found to result in the formation of irregularly shaped platelets of a sodium tungstate rather than nanoparticles of WO₃. Powders of single-phase ZnWO₄ and dual-phase (ZnWO₄)_x(ZnO)_1–x were successfully synthesised by incorporating H₂WO₄ into the ZnCl₂ + Na₂CO₃ + 4NaCl reactant mixture. The photocatalytic activity of these powders was evaluated using the spin-trapping technique with electron paramagnetic resonance spectroscopy. It was found that the photocatalytic activity decreased with the ZnWO₄ content. This decrease in activity was attributed to the larger average particle size of the ZnWO₄ component compared to the ZnO, which reduced the surface area available for interfacial transfer of the photogenerated charge carriers.

Photocatalytic activity of manganese-doped ZnO nanocrystalline powders

ZnO nanocrystalline powders doped with up to 5 at% manganese were synthesized and their photocatalytic activity was studied. Doped ZnO powders were prepared using a sol-gel process. The crystal structure and grain size of the particles were characterized by X-ray diffractometry and optical properties were studied using UV-Vis spectroscopy. The photoactivity of undoped and doped ZnO nanocrystalline powders was evaluated by monitoring the photo-bleaching of the aqueous solutions of Rhodamine B dye in the presence of ZnO under simulated sunlight. The results showed that up to 3 at% manganese were successfully doped into the nanocrystalline ZnO and that manganese-doping reduced the photocatalytic activity of ZnO.

Nanocrystalline zirconia powders synthesised by mechanochemical processing

Mechanochemical processing of zirconium and yttrium chloride precursors with lithium hydroxide has been used to synthesise ultrafine powders of yttria-stabilised zirconia. The precursors reacted during milling to form a composite consisting of nanocrystalline oxide grains embedded within a matrix of lithium chloride. The ultrafine powder was recovered subsequently by removing the lithium chloride through washing with deionised water and methanol. The powders were characterised using X-ray diffraction (XRD), transmission electron microscopy (TEM), and BET gas adsorption. The sintering behaviour of cold pressed pellets was examined by dilatometry.

Synthesis of ultrafine ceria powders by mechanochemical processing

The synthesis of ultrafine cerium dioxide (CeO₂) powders via mechanochemical reaction and subsequent calcination was studied. Anhydrous CeCl₃ and NaOH powders, along with NaCl diluent, were mechanically milled. A solid-state displacement reaction—CeCl₃+ 3NaOH → Ce(OH)₃+ 3NaCl—was induced during milling in a steady-state manner. Calcination of the as-milled powder in air at 500°C resulted in the formation of CeO₂ nanoparticles in the NaCl matrix. A simple washing process to remove the NaCl yielded CeO₂ particles ∼10 nm in size. The particle size was controlled in the range of ∼10–500 nm by changing the calcination temperature.

Process for the production of ultrafine powders

A process for the production of ultrafine powders consisting of individual particles with sizes in the range of 1 nm to 200 nm, which is based on the mechanical milling of two or more non-reacting powders. The process includes subjecting a suitable precursor metal compound and a non-reactant diluent phased to mechanical milling which through the process of mechanical activation reduces the microstructure of the mixture of the form of nano-sized grains of the metal compound uniformly dispersed in the diluent phase. Heat treating the milled powder converts the nano-sized grains of the precursor metal compound into a desired metal oxide phase. Alternatively, the precursor metal compound may itself be an oxide phase which has the requisite milling properties to form nanograins when milled with a diluent. An ultrafine powder is produced by removing the diluent phase such that nano-sized grains of the desired metal oxide phase are left behind. The process facilitates a significant degree of control over the particle size and size distribution of the particles in the ultrafine powder by controlling the parameters of mechanical activation and heat treatment.

Development of a novel micro-spray-assembly process for multilayer ultra-thin film formation

A novel micro-spray-assembly process and an automatic device to fabricate multilayer ultra-thin film are introduced. Employing self-assembly monolayer (SAM) technique, ultra-thin film can be assembled by utilizing the micro-spray-assembly device. The thickness and roughness of each monolayer can be controlled by varying various materials attributes, i.e., deposition time, ionic strength, pH value, molecular concentration and by selecting different manufacturing parameters of the automatic device such as spraying rate, size of micro-drop, N₂ flow rate, temperature of N₂ flow.

Thermal and chemical properties of wool powders

Wool powders with different particle sizes were examined in terms of their crystal structures, thermal properties, surface chemical compositions and moisture regains. It was found that the crystallinity of wool powders was increased, and the moisture regains were decreased as the particle sizes of wool powders were reduced. For comparison, the properties of activated charcoal were also investigated. The higher dye uptake of activated charcoal at pH 10. compared to that of wool powder, could be due to its greater surface area and porous structure.

Wool powders used as sorbents to remove Co2+ ions from aqueous solution

The Co2+ sorption of two wool powders was investigated using its radioisotope 57Co (T1/2=271.8 days and γ=122.1 and 136.5 keV) as a tracer. The effects of the type of buffer, the pH value, the contact time and the initial concentration of Co2+ on the sorption behaviour of wool powders were studied. The Co2+ releasing ability of wool powders and the re-use of wool powders to sorb Co2+ were also examined. The optimum sorption of Co2+ by the powders occurred at pH 8 in phosphate buffer and pH 10 in ammonium sulphate buffer. Fourier-transform infrared spectroscopy (FTIR) was used to study the changes in chemical structure of the wool after exposure to both buffer solutions. Compared to the untreated wool fibre, the fine wool powders showed rapid sorption rates and high sorption capacities for Co2+. Co2+ ions were recovered after exposing the Co2+ loaded wool to HCl (0.1 M) and buffer at pH 3 (glycine/sodium chloride). After releasing Co2+ ions from wool powders, the efficiency of wool powders re-used to sorb Co2+ was 80% of that of the fresh wool powders. It is concluded from this study that wool powder can be used as an efficient sorbent to remove and release Co2+ from solution.

Growth of V2O5 nanorods from ball-milled powders and their performance in cathodes and anodes of lithium-ion batteries

The two-stage procedure of ball milling and annealing in air represents a prospective method of preparing nanorods of V₂O₅ with electrochemical properties suitable for the application in lithium-ion batteries. Commercially purchased V₂O₅ powder is milled in a ball mill as the first step of the synthesis. The as-milled precursor is subsequently annealed in air to produce the morphology of nanorods via solid-state recrystallization. We have recently investigated intermediate stages of the formation of nanorods, and this paper summarizes the synthesis method including the description of the current understanding of the growth mechanism. The obtained V₂O₅ nanorods have been assessed as an electrode material for both anodes and cathodes of lithium-ion batteries. When used in cathodes, the nanorods demonstrate a better retention of capacity upon cycling than that of the commercially available powder of V₂O₅. When used in anodes, the performances of nanorods and the reference V₂O₅ powder are similar to a large extent, which is related to a different operating mechanism of V₂O₅ in anodes. The experimentally observed capacity of V₂O₅ nanorods in an anode has stabilized at the level of about 450 mAh/g after few cycles.

Fabrication of carbon nanofiber by pyrolysis of freeze-dried cellulose nanofiber

The possibility of fabricating carbon nanofibers from cellulose nanofibers was investigated. Cellulose nanofiber of ~50 nm in diameter was produced using ball milling in an eco-friendly manner. The effect of the drying techniques of cellulose nanofibers on the morphology of carbon residue was studied. After pyrolysis of freeze-dried cellulose nanofibers below 600 °C, amorphous carbon fibers of ~20 nm in diameter were obtained. The pyrolysis of oven-dried precursors resulted in the loss of original fibrous structures. The different results arising from the two drying techniques are attributed to the difference in the spatial distance between cellulose nanofiber precursors.