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Compounds of type [(Ph3P)2AgIn(SC(O)R)4] (R = Me (1), Ph (2)) are excellent single-source precursors for AgInS2 bulk materials by pyrolysis and AgIn5S8 films by aerosol assisted chemical vapour deposition (AACVD).
A four-stage sequential extraction procedure for the speciation of nickel has been applied to ambient aerosol samples. The determination of the soluble, sulfidic, metallic and oxidic Ni fractions in particulate matter was carried out by graphite furnace (electrothermal) atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). An EDTA solution, a mixture of diammonium citrate and hydrogen peroxide, and a KCuCl3 solution were used as leaching agents for the determination of the soluble, sulfidic and metallic species, respectively, and nitric acid was used for the determination of oxidic compounds after microwave digestion of particulate matter sampled on filters. A new micro scale filter holder placed in a closed flow injection analysis (FIA) system for use in nickel speciation by means of sequential extraction, and the results of the optimisation of the extraction conditions are described. The temperature program for ETAAS was optimised for all extraction solutions with the aid of temperature curves. Pyrolysis temperatures of 900. 600 and 1,000 degrees C were found to be optimum for EDTA, hydrogen peroxide plus ammonium citrate and KCuCl3-containing solutions, respectively. Airborne dust was sampled on lilters at two locations near to a metallurgical plant in Dortmund, Germany. Concentrations in the low ng m(-3) range down to the detections limits (0.1-0.3 ng m(-3)) and various nickel species were found to be present in the collected dust. The mean fractions of total nickel (sampling period of one month) were found to contain 36+20% of soluble, 6 +/- 4% of sulfidic, 11 +/- 15% of metallic and 48 +/- 18% of oxidic nickel.
Macroporous SiC with a highly ordered pore array was prepared for the first time using low molecular weight SiC preceramic polymers such as polymethylsilane or polycarbosilane by utilizing sacrificial colloidal silica crystalline arrays, as a template which were subsequently etched off after pyrolysis in an argon atmosphere.
A novel nanostructure of Ni nanotubes encapsulated in carbon nanotubes has been obtained via the pyrolysis of C2H2 on an array of Ni nanotubes in an alumina membrane support and a possible mechanism has been proposed.
Polyferrocenylsilane nanorods were prepared using a porous anodic aluminium oxide template followed by chemical etching; pyrolysis was used to obtain magnetic iron oxide-containing ceramic nanorods.
A novel method, combining chemical vapor deposition and pyrolysis of trimethoxyborane under ammonia atmosphere, has been developed to synthesize spherical boron nitride particles with a uniform diameter distribution from 50 to 400 nm; chemical composition and high-resolution transmission electron microscopy analyses indicate that the sub-micron boron nitride particles exhibit a slightly distorted arrangement of the shell layers.
A silicon boron imide based gel Si3B(NH)x(NH2)y(NMe2)z was prepared via catalytic ammonolysis of tris[tris(dimethylamino)silylamino]boron B[HNSi[N(CH3)2]3]3; pyrolysis of the gel under ammonia at 1,000 degrees C gives a mesoporous silicon boron nitride with high surface area and narrow pore size distribution.
The tower-like structure of ZnO nanocolumns grows normal to alumina substrates via pyrolysis and oxidation of ZnS, and is formed by stacking of ZnO nanocrystals layer upon layer.
Octahedral Os(II) complexes 1-5 with formula [Os(CO)3X(dbm)] are prepared through utilization of both solid-state pyrolysis and ligand exchange reactions. These complexes exhibit prominent 3pi-pi* phosphorescence with unusually long lifetimes (29-64 micros) and high quantum yields (0.08-0.13).
Aligned SiC-C coaxial nanocables were synthesized via the direct growth of SiC nanowires from silicon substrates and subsequent carbon deposition using pyrolysis of methane; the average diameter of the SiC nanowire cores is 20 nm; the thickness of the C outer layers is controlled in the range 3-50 nm; the degree of crystalline perfection of the graphitic sheets increases with the thickness.
By pyrolysis of CdS powder in inert gas, single-crystalline cadmium nanotubes growing in the form of a heap, were produced for the first time in high yield.
Sediments from twelve sea lochs on the west coast of Scotland were analysed for parent and branched 2- to 6-ring polycyclic aromatic hydrocarbons (PAHs), n-alkanes and geochemical biomarkers (triterpanes). Where possible at least fourteen sediment samples were collected at random from each sea loch. All sea lochs were remote, most had limited industrial and urban inputs, although all had fish farms. Four lochs had moderate total PAH concentrations and eight lochs had high total PAH concentrations. Total PAH concentration was related to organic carbon content and particle size distribution, with sandier sediments having lower PAH concentrations. The highest total PAH concentrations, normalised for organic carbon, were in Loch Linnhe and Ballachulish Bay (Loch Leven), close to an aluminium smelter. PAH concentration ratios showed that pyrolysis was the main source of PAHs in most lochs. Only sediments from Loch Clash showed evidence of petrogenic input based on their geochemical biomarker (triterpane and sterane) and n-alkane profiles. PAH profiles were similar across lochs apart from Loch Linnhe and Ballachulish Bay, which had a greater proportion of heavy parent PAHs. West coast sediments had a smaller proportion of heavy PAHs than sediments collected from voes in Shetland and a smaller proportion of alkylated PAHs relative to sediments collected from coastal waters around Orkney.
Thin films of a cobalt-clusterized poly(ferrocenylsilane) have been shown to behave as a negative-tone resist for UV photolithography, allowing access to feature sizes between 20 and 300 microm. Pyrolysis of the patterned polymer at 900 degrees C under a N(2) atmosphere afforded patterned ferromagnetic ceramics with excellent shape retention.
Vigorous evaporation of aqueous serine solutions yields abundant protonated serine octamer ions. So does pyrolysis of L-serine crystals in a corona discharge.
La(0.6)Sr(0.4)Co(0.2)Fe(0.8)O(3-delta)(LSCF) perovskite powders have been synthesised by solid-state reaction, co-precipitation, drip pyrolysis and citrate gel routes, and characterised using XRF, XRD, SEM and BET. Co-precipitation using oxalic acid or aqueous ammonia as precipitant failed to achieve the correct chemical composition. Perovskite structures were achieved in all other cases. Surface areas ranging from 0.6 to 17.4 m(2) g(-1) were obtained, which was reflected in the different microstructures observed. The citrate gel product exhibited a convoluted network morphology resulting in its large surface area. Thin-walled (approximately 200 microm) tubular membranes have been manufactured from the LSCF powders using viscous plastic processing. The tubes have been characterised using a custom-built gas analysis rig with on-line mass spectrometry. Porosity levels of the membranes were found to be very low (<0.1%). The spontaneous oxygen flux across the tubular membranes was determined as a function of temperature. Oxygen permeation rates ranged from 0.1 to 0.3 micromol cm(-2) s(-1) at 1273 K. The catalytic behaviour of the LSCF tubes towards methane oxidation has been studied using temperature programmed reaction and conventional catalytic measurements. The tubes favoured combustion reactions, with smaller amounts of partial oxidation and oxidative coupling products observed. Powder coatings have been incorporated to establish the effect of increasing surface area.
Three-dimensional long range ordered hollow SiC and filled SiCN sphere assemblies were prepared for the first time by embedding low molecular weight pre-ceramic polymers of polymethylsilane and polysilazane into sacrificial 3DOM carbon templates which were subsequently burned out in air after pyrolysis under a nitrogen atmosphere.
Iron oxide (Fe(3)O(4), magnetite) nanocrystals of 6 to 30 nm with narrow size distributions (sigma = 5-10%) were prepared by the pyrolysis of iron carboxylate salts.
Self-focusing of intense microwave radiation at the tip of a 25 microm diameter platinum disk microelectrode immersed into the ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM(+)PF(6)(-)) containing 1 mM ferrocene causes dramatically (two orders of magnitude) enhanced voltammetric current signals and temperatures in excess of 600 K (at the electrode surface)--extreme conditions sufficient for condensed phase pyrolysis processes to occur.