The composition of Rhassoul clay is controversial regarding the nature of the pure-mineral clay fraction which is claimed to be stevensite rather than saponite. In this study, the raw and mineral fractions were characterized using various techniques including Fourier transform infrared spectroscopy and magic angle spinning nuclear magnetic resonance (MAS NMR). The isolated fine clay mineral fraction contained a larger amount of Al (>1 wt.%) than that reported for other stevensite occurrences. The 27Al MAS NMR technique confirmed that the mineral is stevensite in which the Al is equally split between the tetrahedral and octahedral coordination sites. The 29Si NMR spectrum showed a single unresolved resonance indicating little or no short-range ordering of silicon. The chemical composition of the stevensite from Jbel Rhassoul was determined to be ((Na0.25K0.20)(Mg5.04Al0.37Fe0.20☐0.21)5.61(Si7.76Al0.24)8O20(OH)4). This formula differs from previous compositions described from this locality and shows it to be an Al-bearing lacustrine clay mineral.

Total neutron scattering measurements, analysed using a modification of the reverse Monte Carlo modelling method to account for long-range crystallographic order, have been used to describe the temperature-dependent behaviour of the structure of quartz. Two key observations are reported. First, the symmetry change associated with the displacive α–β phase transition is observed in both the long-range and short-range structural correlations. Secondly, some aspects of the structure, such as the Si–O bond length and the thermally-induced dynamic disorder, the latter of which sets in significantly below the transition, are relatively insensitive to the phase transition. These results are used to show that the α-domain model of the β-phase disorder is inappropriate and that the classical soft-mode picture of the phase transition is too simplistic. Instead, it is argued that the structural behaviour is best described in terms of its ability to respond to low-frequency, high-amplitude vibrational modes. This view is supported by additional single-crystal diffuse neutron scattering measurements.

Vaterite and aragonite polymorphs in freshwater cultured pearls from mussels of the genus Hyriopsis (Unionidae) were structurally and compositionally characterized by Raman spectroscopy, Micro computer tomography, high resolution field emission scanning electron microscopy, electron microprobe analysis and laser ablation inductively coupled plasma mass spectrometry. The appearance of vaterite in pearls is related to the initial stages of biomineralization, although we demonstrate that vaterite can not be a precursor to aragonite. It is not related to a particular crystal habit and therefore does not have a structural functionality in the pearls. Larger contents of elements typically bound to organic molecules, such as P and S in vaterite, as well as larger total organic contents in vaterite as opposed to aragonite in conjunction with larger concentrations of Mn2+ and Mg2+, imply a stabilizing role of organic macromolecules and X2+ ions for biological vaterite. Distribution coefficients between aragonite and vaterite for provenance-independent elements, such as Mn and Mg (0.27 and 0.04, respectively) agree very well with those observed in fish otoliths.

The solid-state phase transitions of bismuth(III) oxide (Bi2O3) nanoparticles were investigated by complementary methods such as differential scanning calorimetry, differential thermal analysis with combined thermogravimetry and mass spectrometry, and high-temperature x-ray diffraction as compacted nanopowder. At room temperature the particles resided in the β-phase, which is usually a metastable high-temperature phase of bulk Bi2O3. The complementary experimental methods were linked and a nanophase (tetragonal β-phase) → bulk-phase (monoclinic α-phase) transition was identified which was preceded by crystal growth and evaporation of O and C containing species. It was also shown that the atmosphere (more precisely its absolute pressure) has an influence on the transition behavior. An interpretation was proposed that successfully explains all observations from this work and from literature: A sudden destabilization takes place around 735 K due to the loss of the stabilizing, carbonized surface. This leads to the observed transformation to the bulk-phase. But if the particles are smaller than a certain, critical size in the nanorange and are not allowed to grow, they remain in the nanophase until they melt.

Properties of entangled materials, made of fibers, depend on the number and the nature of contacts between fibers and fibers orientation. Nonsintered and sintered steel wools have been characterized by x-ray tomography to extract structural information such as fibers orientation and number of contacts before and during compression. Image analysis techniques were developed on tomography images and validated on virtual materials, generated and deformed by numerical simulation based on molecular dynamic equations. The structural parameters measured during the structural characterization were finally used to link the structure of the studied material with the measured mechanical properties. To do this link, an analytical model usually used for this kind of material was modified to describe the evolution of mechanical properties in compression.

The microstructure of Cu80Fe10Ni10 (at. %) granular ribbons was investigated by means of three-dimensional field ion microscopy (3D FIM). This ribbon is composed of magnetic precipitates embedded in a nonmagnetic matrix. The magnetic precipitates have a diameter smaller than 5 nm in the as-spun state and are coherent with the matrix. No accurate characterization of such a microstructure has been performed so far. A tomographic characterization of the microstructure of melt spun and annealed Cu80Fe10Ni10 ribbon was achieved with 3D FIM at the atomic scale. A precise determination of the size distribution, number density, and distance between the precipitates was carried out. The mean diameter for the precipitates is 4 nm in the as-spun state. After 2 h at 350°C, there is an increase of the size of the precipitates, while after 2 h at 400°C the mean diameter of the precipitates decreases. Those data were used as inputs in models that describe the magnetic and magnetoresistive properties of this alloy.

The ternary alloy GaAlN has been grown by low pressure MOVPE (76 Torr) using triethylgallium, trimetylaluminum and ammonia as precursors. The alloy layers were grown on (0001) sapphire substrates using a low temperature AlN buffer. All layers were deposited at a growth temperature of 980°C. Only the aluminum/gallium ratio in the gas phase was changed, keeping the total group III molar flow rate and V/III molar ratio constant.

The aluminum incorporation versus gas phase composition was determined experimentally, using energy dispersive analysis of X-rays (EDAX), and X-ray diffraction. We propose a model, taking into account kinetically limited mass transport of group III species in the gas phase, which describes well the data.

The structural quality of the layers was investigated using X-ray diffraction and TEM experiments.

A degradation of the materials quality is observed with increasing Al content. In this case, growth originate on the buffer grains facets resulting in a “ two directional » growth. This phenomenon, being markedly enhanced when increasing the Al content will be detailed in this paper.