Influence of hydrogen peroxide in the preparation of nanocrystalline ceria

The influence of H2O2 in the preparation of nanocrystalline CeO2 has been investigated by treating solutions of Ce(III) with NaOH in the presence of different concentrations of H2O2. The resulting precipitated material was then examined by a range of techniques, including transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). A decrease in CeO2 crystallite size with increasing H2O2 concentration was observed. This was found to be associated with the formation of an amorphous material containing an η2-peroxide (O22-) species.

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.

Crystal orientation characterisation of electrodeposited nanocrystalline nickel alloy

The collection contains EBSD maps of annealed nanocrystalline Ni and Ni-Fe alloys. The maps show the variation of crystallographic texture across mesoscale colonies within these alloys.

Synthesis and characterization of nanocrystalline hexagonal boron carbo-nitride under high temperature and high pressure

A study of the synthesis of hexagonal boron carbo-nitride (h-BCN) compounds via a two-step high-temperature and high-pressure (HTHP) technique using melamine (C 3N 6H 6) and boron oxide (B 2O 3) as raw materials is presented. An amorphous BCN precursor was prepared at 1000K under vacuum in a resistance furnace and then single-phase h-BCN nanocrystalline was synthesized at 1600K and 5.1GPa in a multi-anvil apparatus. X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the final products were pure h-BCN crystals with the lattice constants a ≤ 0.2510nm and c ≤ 0.6690nm. The average grain size was about 150nm. X-ray photoelectron spectroscopy (XPS) results confirmed the occurrence of bonding between C-C, C-N, C-B and N-B atoms. Raman scattering analysis suggested that there were three strong Raman bands centered at 1359, 1596 and 1617cm -1, respectively. The band at 1617cm -1 was considered to be consistent with the characteristic Raman peak of h-BCN.

Application of white-beam X-ray microdiffraction for the study of mineralogical phase identification in ancient Egyptian pigments

High-brightness synchrotron X-rays together with precision achromatic focusing optics on beamline 7.3.3 at the Advanced Light Source have been applied for Laue microdiffraction analysis of mineralogical phases in Egyptian pigments. Although this task is usually performed using monochromatic X-ray diffraction, the Laue technique was both faster and more reliable for the present sample. In this approach, white-beam diffraction patterns are collected as the sample is raster scanned across the incident beam (0.8 µm × 0.8 µm). The complex Laue diffraction patterns arising from illumination of multiple grains are indexed using the white-beam crystallographic software package XMAS, enabling a mineralogical map as a function of sample position. This methodology has been applied to determine the mineralogy of colour pigments taken from the ancient Egyptian coffin of Tjeseb, a priestess of the Apis bull dating from the Third Intermediate to Late period, 25th Dynasty to early 26th Dynasty (747 to 600 BC). For all pigments, a ground layer of calcite and quartz was identified. For the blue pigment, cuprorivaite (CuCaSi4O10) was found to be the primary colouring agent with a grain size ranging from ∼10 to 50 µm. In the green and yellow samples, malachite [Cu2(OH)2CO3] and goethite [FeO(OH)] were identified, respectively. Grain sizes from these pigments were significantly smaller. It was possible to index some malachite grains up to ∼20 µm in size, while the majority of goethite grains displayed a nanocrystalline particle size. The inability to obtain a complete mineralogical map for goethite highlights the fact that the incident probe size is considerably larger than the grain size. This limit will continue to improve as the present trend is toward focusing optics approaching the diffraction limit (∼1000× smaller beam area).