The Effect of the Rate of Precursor Production on the Purity and Aggregation

The synthesis of zinc oxide through the decomposition of a solid oxalate precursor was investigated. It was found that the rate of preparation of the precursor had a quantitative effect on the morphology and extent of surface ligation of particles produced; contrary to our expectations,it was found that the slow combination of reagents led to a less pure product. It has been determined that this time dependence mimics the variation of reactant ratios. Zinc oxide particles were produced from a number of reactant ratios, and were characterised by TEM, XRD, FT-IR and DSC. It was found that the size of the crystallites produced was not affected, but that the nature of their surface ligation did rely upon these parameters

Self-assembled arrays of ZnO nanoparticles and their application as varistor materials

Linear arrays of ZnO nanoparticles have been successfully prepared by a simple sol–gel condensation reaction involving chemical modifiers, followed by drying (80oC) and calcination (500 oC). The calcined material (nanoarray ZnO) is composed of approximately spherical nanoparticles of average diameter 21+/-3 nm, selfassembled to form arrays extending in length to 2–4 mm. The morphology of the ZnO is found to depend sensitively on the amounts of chemical modifiers present. In their absence the ZnO produced (nano-ZnO) is an unstructured agglomerate of nanoparticles. The mechanism for formation of these linear arrays has been investigated by examining the intermediates formed at 80 oC and 250 oC using XRD and TEM and by following the decomposition reactions using TGA and DSC. Varistors prepared from the nano-array ZnO by sintering (1050 oC) with ppropriate mixtures of metal oxides showed a breakdown voltage of 786 +/- 30 Vmm-1, which is substantially higher than that of samples prepared under similar conditions from either micronsized commercial ZnO (507 +/-30 V mm-1) or from nano-ZnO (683 +/-30 V mm-1)

Self-assembled arrays of ZnO nanoparticles and their application as varistor materials

Linear arrays of ZnO nanoparticles have been successfully prepared by a simple sol–gel condensation reaction involving chemical modifiers, followed by drying (80oC) and calcination (500 oC). The calcined material (nanoarray ZnO) is composed of approximately spherical nanoparticles of average diameter 21+/-3 nm, selfassembled to form arrays extending in length to 2–4 mm. The morphology of the ZnO is found to depend sensitively on the amounts of chemical modifiers present. In their absence the ZnO produced (nano-ZnO) is an unstructured agglomerate of nanoparticles. The mechanism for formation of these linear arrays has been investigated by examining the intermediates formed at 80 oC and 250 oC using XRD and TEM and by following the decomposition reactions using TGA and DSC. Varistors prepared from the nano-array ZnO by sintering (1050 oC) with ppropriate mixtures of metal oxides showed a breakdown voltage of 786 +/- 30 Vmm-1, which is substantially higher than that of samples prepared under similar conditions from either micronsized commercial ZnO (507 +/-30 V mm-1) or from nano-ZnO (683 +/-30 V mm-1)

An Effective Method for the Preparation of High Temperature Stable Anatase TiO2 Photocatalysts

An efficient, rapid and straightforward method for the preparation of nitrogen and fluorine (N, F) codoped high temperature stable anatase using a microwave pre-treatment is reported. Using a single source, ammonium fluoride (NH4F) for both nitrogen and fluorine, effective doping of the precursor titanium isopropoxide (TTIP) was possible. These samples were characterised for their structural and optical properties using X-ray diffraction (XRD), Fourier transform IR (FTIR), Raman spectroscopy and UV-vis spectroscopy. In terms of the anatase to rutile transition enhancement using a novel microwave assisted technique, the sample prepared in a composition of 1:8 TiO2: NH4F at 1200 °C was seen to be most effective, having stable anatase present at 57.1 % compared to undoped TiO2 being 100 % rutile from 900 °C. This method involves the production of ammonium oxofluorotitanates (NH4TiOF3) at low temperatures. The inclusion of these intermediates greatly reduces the particle size growth and delays the anatase to rutile transition. The photocatalytic activity of these materials was studied by analysing the degradation of an organic dye, rhodamine 6G as a model system and the rate constant was calculated by pseudo-first-order kinetics. These results showed that the doped sample (0.0225 min-1) was three times more active than the undoped sample (0.0076 min-1) and over seven times faster than the commercial TiO2 photocatalyst standard Degussa P-25 calcined at 1200 °C (0.0030 min-1). The formation of intermediate compounds, oxofluorotitanates, was identified as the major reason for a delay in the anatase to rutile transition

High Performance ZnO Varistors Prepared From Nanocrystalline Precursors for Miniaturised Electronic Devices

An industrially viable solution-based processing route using minimal amounts of solvent has been used to prepare bulk quantity nanopowders (average particle size 15.3 nm) for the fabrication of ZnO varistors. The xerogels, calcined powders and sintered materials were fully characterised. The preparation of varistors from nanopowders has been optimised by studying the effect of temperature on grain growth, densification and breakdown voltage. The varistors are prepared by sintering at 1050 C for 2 hours, a temperature that is significantly lower than that used in the current industrial process. Highly dense varistor discs prepared from the sintered material produce devices, with a breakdown voltage 85% higher than that of commercial varistors, making them suitable for use in miniaturised electronic circuitry. Improved performance of these materials has been attributed to the small grain size and better dispersion of additives on ZnO grains

An Effective Method for the Preparation of High Temperature Stable Anatase TiO2 Photocatalysts

An efficient, rapid and straightforward method for the preparation of nitrogen and fluorine (N, F) codoped high temperature stable anatase using a microwave pre-treatment is reported. Using a single source, ammonium fluoride (NH4F) for both nitrogen and fluorine, effective doping of the precursor titanium isopropoxide (TTIP) was possible. These samples were characterised for their structural and optical properties using X-ray diffraction (XRD), Fourier transform IR (FTIR), Raman spectroscopy and UV-vis spectroscopy. In terms of the anatase to rutile transition enhancement using a novel microwave assisted technique, the sample prepared in a composition of 1:8 TiO2: NH4F at 1200 °C was seen to be most effective, having stable anatase present at 57.1 % compared to undoped TiO2 being 100 % rutile from 900 °C. This method involves the production of ammonium oxofluorotitanates (NH4TiOF3) at low temperatures. The inclusion of these intermediates greatly reduces the particle size growth and delays the anatase to rutile transition. The photocatalytic activity of these materials was studied by analysing the degradation of an organic dye, rhodamine 6G as a model system and the rate constant was calculated by pseudo-first-order kinetics. These results showed that the doped sample (0.0225 min-1) was three times more active than the undoped sample (0.0076 min-1) and over seven times faster than the commercial TiO2 photocatalyst standard Degussa P-25 calcined at 1200 °C (0.0030 min-1). The formation of intermediate compounds, oxofluorotitanates, was identified as the major reason for a delay in the anatase to rutile transition

New approach of modifying the anatase to rutile transition temperature in TiO2 photocatalysts

In pure synthetic titanium dioxide, the anatase to rutile phase transition usually occurs between the temperatures of 600 °C and 700 °C. The phase transition temperature can be altered by various methods, including modifying the precursor or by adding dopant or modifier to the TiO2 sample. In an attempt to investigate the phase transition using aromatic carboxylic acids, the current study examines the impact of increasing concentrations of benzoic acid (1 : 0, 1 : 1, 1 : 4 and 1 : 8 molar ratio TiO2 : benzoic acid) on anatase to rutile transition. The samples were characterised using Raman spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) studies. At 500 °C, all samples contained only anatase. At 600 °C, the 1 : 1, 1 : 4 and 1 : 8 samples contain only anatase and the control (which contains no modifier) was a mixture of 27% anatase and 73% rutile. At 700 °C, the 1 : 1 molar ratio sample contained 50% anatase/rutile, 1 : 4 and 1 : 8 molar ratio samples were observed to have a majority of anatase, 76% and 71% respectively. When the temperature was increased to 800 °C, the sample with the 1 : 4 molar ratio contained 10% anatase and at the same temperature the 1 : 8 ratio sample contained 7% anatase; the remaining samples (1 : 0 and 1 : 1) at this temperature contained only rutile. These results show that there is a significant % anatase still present when the doped samples were calcined to 700 °C when compared with the control (100% rutile). There are small amounts of the anatase phase in the 1 : 4 and 1 : 8 samples at 800 °C. Therefore, benzoic acid has induced a delay in the rutile formation

Silver Doped Perfluoropolyether-Urethane Coatings: Antibacterial Activity and Surface Analysis

The colonisation of clinical and industrial surfaces with pathogenic microorganisms has prompted increased research into the development of effective antibacterial and antifouling coatings. There is evidence that implanted biomedical surfaces coated with metallic silver can be inactivated by hysiological fluids, thus reducing the bioactivity of the coating. In this work, we report the biofilm inhibition of Staphylococcus epidermidis using a roomtemperatureprocessedsilver dopedperfluoropolyether-urethane coating. The release of silver ions from these fluoropolymers over a six-day period inhibited bacterial encrustation – as observed by scanning electron microscopy (SEM). X-ray photoelectron spectroscopy (XPS) analysis indicated differences in carbon, fluorine and sodium surface composition between silver doped and undoped fluoropolymers after exposure to nutrient rich media. These silver doped perfluoropolyether coatings also exhibited antibacterial activity against methicillin-resistant Staphylococcus aureus (MRSA), Escherichia coli, Pseudomonas aeruginosa and Acinetobacter baumannii; suggesting potential use in preventing transmission of pathogenic and opportunistic microbes on environmental surfaces in healthcare facilities. The broad-spectrum antibacterial activity of these silver release coatings may be exploited on biomaterials surfaces to combat the development of resistant Gram-negative Enterobacteriaceae that can occur during prophylactic treatment for urinary tract infections