Thermal stability of ultrasoft Fe–Zr–N films

The thermal stability of nanocrystalline ultrasoft magnetic (Fe98Zr2)1−xNx films with x = 0.10–0.25 was studied using thermal desorption spectrometry, positron beam analysis and high resolution transmission electron microscopy. The results demonstrate that grain growth during the heat treatment is accompanied by an increase of the free volume and nitrogen relocation and desorption. All these phenomena can drastically degrade the ultrasoft magnetic properties. The nitrogen desorption has already started at temperatures around 400 K. Nevertheless, most of the nitrogen leaves the sample at a temperature above 800 K. We found that nitrogen out-diffusion is significantly retarded compared with the prediction of the diffusion in bulk α-Fe. A qualitative model is proposed in which the nitrogen out-diffusion in nanocrystalline material is retarded by trapping at immobile defects, namely Zr atoms, and also by voids at grain boundaries. From a certain temperature, nitrogen migrates from the interior of the nanograins to the nanovoids at the grain boundaries and the out-diffusion to the outer surface is controlled by transport between the voids.

Catalytic carbonization of wood charcoal:graphite or diamond?

We report on the process of making graphite out of wood by catalytic carbonization. Two different types of microstructure were observed. One type being typical for graphitization of wood without the effect of a catalyst, the main characteristic being the typical fibrillar microstructure related back to the original cellulose morphology. A strong {0002} inner diffraction ring corresponding to the 0.336 nm lattice spacing of graphite dominates its diffraction pattern. The other type being typical for graphitization of wood with aluminum as catalyst, the main characteristic being the large sheets of carbon forced upon by the formation of plate like Al4C3. This compound is formed as an intermediate reaction product, which dissociates into aluminum vapour and solid carbon. The diffraction pattern indicates a differently textured structure. EELS measurements in the areas of catalytic graphitization indicate a significant decrease of the sp(2) bonding typical for graphite. It can be an indication of the presence of metastable diamond. This diamond-like structure is extremely unstable under influence of the electron beam. It decomposed within 250 s of beam exposure. (C) 2003 Elsevier Ltd. All rights reserved

Secondary electron spectra of semi-crystalline polymers – a novel polymer characterisation tool?

The nano-scale dispersion of ordered/disordered phases in semi-crystalline polymers can strongly influence their performance e.g. in terms of mechanical properties and/or electronic properties. However, to reveal the latter in scanning electron microscopy (SEM) often requires invasive sample preparation (etching of amorphous phase), because SEM usually exploits topographical contrast or yield differences between different materials. However, for pure carbon materials the secondary spectra were shown to differ substantially with increased order/disorder. The aims here is to gain an understanding of the shape of secondary electron spectrum (SES) of a widely used semi-crystalline polymer regioregular poly(3-hexylthiophene-2,5-diyl), commonly known as P3HT, and its links to the underlying secondary electron emission mechanisms so SES can be exploited for the mapping the nanomorphology. The comparison of simulated and experimental SES shows an excellent agreement, revealing a peak (at about 0.8eV) followed by a broad shoulder (between 2eV and 4.5eV) with respective relative intensities reflecting order/disorder