Crystallization of some anorthite-diopside glass precursors

Anorthite and diopside have been obtained from complete devitrification of glasses belonging to the quaternary system MgO-CaO-Al₂O₃-SiO₂. Microstructure, the natural trend of the nucleation mechanism and kinetic studies on the crystallization phenomenon have been investigated by means of optical and electron microscopies, thermal and thermomechanical techniques and X-ray powder diffractometry. All the glasses investigated show a complete crystallization starting from a simple surface nucleation process. The activation energy for the crystallization process proved to be higher than that for viscous flow, leading to an important aspect modification in the sample during ceramization. Thermal stability and physical properties of both glass and glass-ceramic materials have been tested, suggesting the possible use of these materials in industrial application.     

Antimutagenic activity of phenolic compounds, oligosaccharides and quinolizidinic alkaloids from Lupinus campestris seeds.

There are some foods that contain mutagenic or carcinogenic agents, some of which occur naturally and others that may be formed during preparation or cooking. Several foods such as legumes, also contain natural antimutagens and/or anticarcinogens. Lupine is one such legume that contains high amounts of protein (40%) and oils (14%). About 90 species of lupine have been reported throughout Mexico. However, the use of this crop as a source of food has been limited by the presence of antinutritional agents such as phenolic compounds (PC), carbohydrates (CH) and quinolizidinic alkaloids (Qas). It has also been suggested that consuming these compounds can affect human health and may even reduce the risk of disease. The objective of this work was to determine the effect of PC, CH and Qas, isolated and quantified from Lupinus campestris on the mutagenicity of 1-nitropyrene (1-NP) as a model mutagen and we used the Salmonella typhimurium tester strain YG1024 by the Kado microsuspension method. The results indicate that L. campestris seeds have 11 mg (+)catechin equivalent g(-1) seed coat; 120.3 mg g(-1) seeds and 2.13 mg g(-1) seeds of PC, CH and Qas, respectively. 1-NP mutagenicity was inhibited by 86% for PC, 76% for CH and 75% for Qas at concentrations of 200, 512 and 13.6 microg/tube, respectively.     

LLDPE’s grown with Metallocene and Ziegler–Natta catalysts: events in the melt and FTIR analysis

LLDPE samples synthesized with Ziegler–Natta (ZN) and Metallocene (MT) catalysts have been analyzed to investigate a potential catalyst-dependent morphology and to find an explanation for the difficult processing of MT. Slow calorimetry at v = 0.02 K/min and IR at RT and in the melt are used. The differences between MT and ZN are assigned to their different composition, MT not having the linear segments, which are present in ZN. Slow calorimetry is effectively a drawing process of the melt with chain orientation followed by decay. The later event, characterized by an endotherm, ΔH _network, occurs at higher temperatures for MT, the presence of a regular distribution of methyl groups slowing down the process. The rocking, gauche, bending and stretching regions of the IR spectra are analyzed. The nascent MT has more strained bands in the rocking region. The wagging region reveals the more homogeneous environment of MT through the maximum absorbance at 1,368 cm⁻¹. Decomposition of bands is made for the rocking and wagging regions. The orthorhombic crystallinity, α_c (FTIR), measures the sum of long- and short-range orthorhombic order, the latter being obtained by α_c (FTIR)-α_c (X-rays). The values of α_c (FTIR) for MT and ZN are very similar in conditions of equilibrium. The justifications for the molecular origin of ΔH _network are presented: (i) the slow relaxation of long chains strained and oriented in the melt measured by other techniques, (ii) The correlation, for gels of a linear sample, made in different solvents, between the maximum drawability, λ_max, and ΔH _network in a slow T-ramp. The range is 80–270 for λ_max and 40–120 J/g for ΔH _network. (iii) The comparison of two traces of the same sample, between 140 °C and 270 °C, show that comparable events in the melt appear in the integrated absorbance and in the slow calorimetry signal. Analysis on thin films of the little-studied CH₂ stretching region reveals that their extinction coefficient, ε, and the shape of the bands are highly sensitive to the sample history, ε diminishing by a large factor in slowly crystallized samples. Events in the slow T-ramp, followed by a fast crystallization, on the other hand, leads to materials with standard characteristics. Slow calorimetry traces display more events (endothermic and exothermic) for MT than for ZN, a finding consistent with more flow irregularities during processing. Equilibrium conditions and better processing could be reached for MT by extending time in the melt or using higher temperatures.     

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.     

The hypersonic environment: Required operating conditions and design challenges

Hypersonic flight powered by airbreathing engines offers the potential for faster response time at long ranges, and reduced cost for access-to-space. In the present paper the operating environment of typical hypersonic vehicles are discussed, including results for the radiation equilibrium wall temperature of external vehicle surfaces and the flow properties through three sample engines spanning the range of hydrocarbon-fueled Mach 4-8 flight and hydrogen-fueled flight at speeds up to Mach 17. Flow conditions at several locations through the sample engines were calculated to provide indications of the required operating flow environment. Additional system consideration such a seals, joints, vehicle integration and in-service engineering are addressed.     

Mechanism of thermochemical growth of iron borides on iron

The mechanism of thermochemical growth of iron borides on iron was studied by analysing the products which form on samples placed in contact with B₄C-base powder mixtures with different boronising potential. The analyses were carried out by means of metallographic and X-ray diffraction techniques. Three subsequent stages of growth were observed which explain the occurrence of typical properties of the thermochemically grown boride coatings, such as preferred crystallographic orientations and textures, as well as mechanical compactness and hardness, which play a determining role in the tribological behaviour of borided components.     

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.