Probing the thermal decomposition process of layered double hydroxides through in situ <Superscript>57</Superscript>Fe Mössbauer and in situ X-ray diffraction experiments

The thermal decomposition properties of Mg–Fe hydrotalcites were studied through in situ ⁵⁷Fe Mössbauer spectroscopy and in situ X-ray diffraction. Abrupt changes in the quadrupolar splitting measured in the Mössbauer spectra revealed a phase transition from the starting lamellar structure to a new crystalline arrangement. By analyzing the Mössbauer parameters we show that the material is highly disordered in the 300–400 °C temperature range. This hypothesis is confirmed by the X-ray results whose diffractograms indicated the collapse of the lamellar structure and the formation of a solid solution.     

Modelling of effects of ultrastructural morphology on the hygroelastic properties of wood fibres

Wood fibres constitute the structural framework of e.g. wood, paper, board and composites, where stiffness and dimensional stability are of importance. An analytical modelling approach has been used for prediction of hygroelastic response, and assessment of the stresses in thick-walled cylinder models of wood fibres. A wood fibre was idealised as a multilayered hollow cylinder made of orthotropic material with helical orientation. The hygroelastic response of the layered assembly due to axisymmetric loading and moisture content changes was obtained by solving the corresponding boundary value problem of elasticity. A simple solution scheme based on the state space approach and the transfer matrix method was employed. This was combined with an analytical ultrastructural homogenisation method, used to link hygroelastic properties of constituent wood polymers to properties of each layer. Predicted hygroelastic response captured experimentally measured behaviour. Fibres that were constrained not to twist showed a stiffer response than fibres allowed twisting under uniaxial loading. It was also shown that the ultrastructure, i.e. the microfibril angle, will control the hygroexpansion in the same way as it controls the compliance of the cell wall. Qualitative failure trends comparable with experimental observations could be established with stress analysis and a simple plane-stress failure criterion.     

Dielectric and thermal characteristics of gel grown single crystals of ytterbium tartrate trihydrate

Dielectric and thermal characteristics of gel grown single crystals of ytterbium tartrate trihydrate have been carried out. The dielectric constant has been measured as a function of frequency in the range 2 kHz–1 MHz and temperature range 30–300 °C. The dielectric constant increases with temperature, attains a peak near 215 °C, and then decreases as the temperature exceeds 215 °C. The dielectric anomaly at 215 °C is suggested to be due to phase transition brought about in the material. The dielectric behaviour of the material is correlated with the results on thermal analysis. Thermogravimetric and differential thermal analysis have been used to study the thermal characteristics of the material. The experimental results show that the material is thermally stable up to 200 °C. The decomposition process occurs in two stages until ytterbium oxide is formed at 700 °C. The non-isothermal kinetic parameters e.g., activation energy and the frequency factor have been evaluated for each stage of thermal decomposition by using the integral method, applying the Coats–Redfern approximation.     

Hydrogen adsorption studies in micro-size cobalt dots

Hydrogen desorption curves were obtained from a sample composed of a square arrangement of Co dots with average diameter of 4.4 μm, separated by a distance of 11.6 μm. A macroscopic sample of Co dots grown on a 2.5 × 2.5 cm Si substrate was made by standard lithographic techniques and used in these experiments. Thermal programmed desorption (TPD) was performed under ultra-high vacuum conditions. Hydrogen TPD curves were obtained from a 1 × 1 cm Co dots samples displaying a maximum of intensity at 425 K. Hydrogen TPD curve was also obtained from 1 cm× 1 cm samples of Co films and Co foils for comparison. The hydrogen TPD curves have decreasing intensity from the Co foils to the Co dots and finally to the Co films. This indicates that there are more sites for hydrogen adsorption on the Co dots than in the Co films. This is a surprising result because there is approximately 8.7 times less Co atoms exposed in the Co dots that in the Co film sample. A desorption energy of 27 kcal/mol was obtained for the Co dots suggesting that hydrogen is adsorbed on an hcp hollow site of the Co dot crystalline structure.     

A review on the synthesis of in situ aluminum based composites by thermal,mechanical and mechanical–thermal activation of chemical reactions

The aim of the present paper is to review the recent progress in the synthesis of in situ particle reinforced aluminum composites using thermal, mechanical and combined mechanical-thermal activation of aluminothermic reduction reactions. The combination of combustion synthesis (CS) and mechanosynthesis (MS) is the most recent development in the processing of advanced materials like micro and nano aluminum based composites. The combined mechanical thermal synthesis (MTS) has widened the possibilities for both CS and MS. MTS holds great potential for commercial viability and offers exciting processing route for the synthesis of advanced materials. Enhanced reaction kinetics and extended concentration limits in MTS are demonstrated by illustrating the synthesis of aluminum based nanocomposite involving Al–CeO₂.     

Dissolution processes,hydrolysis and condensation reactions during geopolymer synthesis: Part I—Low Si/Al ratio systems

Initial geopolymeric reaction processes governing dissolution of solid aluminosilicate particles in alkali solutions have been investigated using conventional experimental techniques, and the data analysed by speciation predictions of the partial charge model (PCM). For metakaolin powders activated with 5.0 M NaOH, solid-state nuclear magnetic resonance (NMR) spectra disclose the existence of monomeric [Al(OH)₄]⁻ species after two hours of dissolution, consistent with PCM predictions. However, no equivalent monomeric silicate species were observed for 5.0–10.0 M NaOH activator solutions characteristic of systems with nominal Si/Al ≤ 1. The apparent absence of monomeric silicate species suggest rapid condensation of silicate units with [Al(OH)₄]⁻ to generate aluminosilicate species, as indicated by the evolution of the shoulder at around −87 ppm in the ²⁹Si NMR spectra. Of the two possible stable silicate species [SiO₂(OH)₂]²⁻ and [SiO(OH)₃]⁻, the latter appears most likely to condense with [Al(OH)₄]⁻ to produce aluminosilicate oligomers, from which larger oligomers subsequently form through further condensation with [Al(OH)₄]⁻ leading to a gradual build up of aluminosilicate networks and a lowering of system alkalinity. This dissolution and hydrolysis sequence at the early stages of synthesis suggests a reaction path wholly consistent with predictions of the partial charge model.     

Surface barrier diode based on zinc selenide with a passivating zinc oxide film

We propose a method of fabricating surface barrier diodes with overlapped metal junction, which provides for a significant decrease in the reverse currents and an increase in the breakdown voltage.     

An analysis of nonlinear ion drift spectrometry for gas detectors with separating chamber of planar geometry

A consistent analytical model of nonlinear ion drift spectrometry for modern gas analyzers is developed. A procedure for determining the field dependence of the ion mobility using the experimental data is described. An ionogram is calculated for the case of a flat drift chamber and polynomial character of the field dependence of the ion mobility.     

An in situ TEM study of phase formation in gold-aluminum couples

In the gold wire bonding of aluminum in microelectronic devices the presence of aluminum oxide on the metallization surface may be expected. Electron transparent couples containing an oxide layer at the interface were heated in a TEM to determine the effects of a passivation layer on intermetallic formation. Intermetallic phases were evidenced by changes in sample appearance and their structure was determined by electron diffraction. The presence of an oxide at the interface hindered second phase formation at temperatures at which they were usually expected to form. In aluminum rich couples, the formation of the AuAl₂ intermetallic was not observed to form until about 350°C with the oxide present. In a reverse configuration involving a gold rich couple, an amorphous oxide phase was observed between the Al and the advancing Au₂Al front. The movement of the reaction front appeared to be controlled by surface diffusion across this phase.