Fe/AlOOH gels calcined and reduced at different temperatures have been investigated by a combined use of Mössbauer spectroscopy, x-ray diffraction, and electron microscopy in order to obtain information on the nature of the iron species formed as well as the various reduction processes. Calcination at or below 1070 K mainly gives reducible Fe3+ while calcination at higher temperatures gives substitutional Fe3+ in the form of Al2−xFexO3. The Fe3+ species in the calcined samples are, by and large, present in the form of small superparamagnetic particles. Crystallization of Al2O3 from the gels is catalyzed by Fe2O3 as well as FeAl2O4. Fe (20 wt. %)/AlOOH gels calcined at or below 870 K give FeAl2O4 when reduced in hydrogen at 1070 K or lower and a ferromagnetic Fe0–Al2O3 composite (with the metallic Fe particles >100 Å) when reduced at 1270 K. Samples calcined at 1220 K or higher give the Fe0–Al2O3 composite when reduced in the 870–1270 K range, but a substantial proportion of Fe3+ remains unreduced in the form of Al2−xFexO3, showing thereby the extraordinary stability of substitutional Fe3+ to reduction even at high temperatures. Besides the ferromagnetic Fe0–Al2O3 composite, high-temperature reduction of Al2−xFexO3 yields a small proportion of superparamagnetic Fe0–Al2O3 wherein small metallic particles (<100 Å) are embedded in the ceramic matrix. In order to preferentially obtain the Fe0–Al2O3 composite on reduction, Fe/AIOOH gels should be calcined at low temperatures (∼1100 K); high-temperature calcination results in Al2−xFexO3. Several modes of formation of FeAl2O4 are found possible during reduction of the gels, but a novel one is that involving the reaction, 2Fe3+ + Fe0 → 3Fe2+.

Twenty-five silicates were irradiated at ambient temperature conditions with 1.5 MeV Kr+. Critical doses of amorphization were monitored in situ with transmission electron microscopy. The doses required for amorphization are compared with the structures, bond-types, compositions, and physical properties of the silicates using simple correlation methods and more complex multivariate statistical analysis. These analyses were made in order to determine which properties most affect the critical amorphization dose. Simple two-variable correlations indicate that melting point, efficiency of atomic packing, the dimensionality of SiO4 polymerization (DOSP), and bond ionicity have a relationship with critical amorphization dose. However, these relationships are evident only in selected portions of the data set; that is, for silicate phases with a common structure type. A clearer relationship between the silicate properties and critical amorphization dose was determined for the entire data set with multiple linear regression. Several regression models are proposed which describe the variation in amorphization dose. All regression models contain the following properties: (i) melting point; (ii) a structural variable (DOSP, elastic modulus, and/or atomic packing); and (iii) the proportion of Si–O bonding (instead of bond ionicity). The regression models are equivalent, because they represent combinations of similar properties. Notably, density and atomic mass are not controlling properties for the critical amorphization dose. Melting and amorphization by ion irradiation are apparently related processes. Neither melting point nor critical amorphization dose can be predicted by considering only the structure, composition, or bonding of a particular phase. The Si–O bond is the most covalent bond in silicates, and is the “weak link” in the structure with respect to amorphization. Thus, DOSP is also an important property, as the topology of these “weak links” influences a structure's ability to accumulate amorphous regions. The efficiency of atomic packing is related to the process of defect self-recombination during amorphization. The bulk modulus and shear modulus are important variables within the regression models because of their direct relationship to atomic packing.

Kinetics of cristobalite precipitation in a binary glass composite, containing a low-softening borosilicate (BSG) and a high-softening high silica (HSG) glass, have been investigated. XRD results show that the pure glasses do not crystallize under the sintering conditions used, but when mixed in appropriate proportions the cristobalite gradually precipitates out of the initial amorphous binary glass mixture as the sintering continues at temperatures ranging from 800 to 1000 °C. Average linear thermal expansion coefficient (TCE) results show that the TCE increases significantly with increasing precipitation of cristobalite as a function of sintering time. Comparing the experimental TCE results with those theoretically calculated, it is concluded that the precipitation originates most likely in the HSG rather than in the BSG. The precipitation kinetics follow the Avrami equation, and the results show an apparent activation energy of 82 kJ/mol which is close to those for the diffusion of alkali ions in silicate glasses, suggesting mass-transport controlled kinetics. The values of the Avrami exponent are 1.7–1.8, which could be interpreted as a 3-dimension diffusional growth at zero nucleation rate. The linear growth rates of cristobalite, calculated from the precipitation curve, are in the range of 4–8 × 10−5 μm/min, and show slight temperature dependence from 800 to 1000 °C. The linear growth rates of cristobalite are also calculated theoretically using the equation derived by Turnbull et al.,2 and the data are 0–3 orders of magnitude smaller than those observed experimentally. This disparity is attributed to the catalytic effect of the OH and O in air and in the glass network, as well as the diffusion of alkali ions from BSG to HSG.

An apparatus was constructed that measured hardness under load. The instrument measured hardness using a strain-gauge load cell and a linear voltage displacement transducer. Loading rates were less than 1 μm/s. Results were similar to the results of other electronic hardness measurement devices, in that the hardness fell with increasing load. Glasses measured have Meyers indexes from 1.6 to 1.75, while polycrystalline materials showed much more complex behaviors. A model was formulated to explain the data for glasses based on expansion of shear planes.

A discrete model of springs with bond-bending forces is proposed to simulate the fracture process in a composite of short stiff fibers in a softer matrix. Both components are assumed to be linear elastic up to failure. We find that the critical fiber length of a single fiber composite increases roughly linearly with the ratio of the fiber elastic modulus to matrix modulus. The finite size of the lattice in the direction perpendicular to the fiber orientation considerably alters the behavior of the critical length for large values of the modulus ratio. The simulations of the fracture process reveal different fracture behavior as a function of the fiber content and length. We calculate the Young's modulus, fracture stress, and the strain at maximum stress as a function of the fiber volume fraction and aspect ratio. The results are compared with the predictions of other theoretical studies and experiments.

The incorporation of ductile fibers in brittle matrices can lead to a significant increase in fracture resistance. The increase in toughness that derives from crack bridging is governed by the properties of the matrix/fiber interface and the ductility of the fibers. The current study addresses the role of interface sliding stress on the toughness of brittle composites reinforced with ductile fibers. The debond length is explicitly related to the interface sliding stress and the properties of the fiber. It is then incorporated into a geometrical model to simulate the bridging tractions versus crack opening under condition of continuous debonding. The implications on the effect of interfaces on the resistance curve are discussed.

The transfer of polytetrafluoroethylene (PTFE) onto stainless steel (AISI 316) and silicon wafers in a static contact was characterized at temperatures ranging from 21 °C to 300 °C. The amount of transferred PTFE on AISI 316 substrate was found to be strongly time- and temperature-dependent, and reached a steady state after a certain period of contact time. On testing the effect of temperature on this steady transfer state, an almost temperature independent amount of PTFE was observed to be transferred onto AISI 316 at temperatures between 130 and 180 °C. This steady state started at the glass transition at about 127 °C. This was significantly consistent with an almost constant amorphous-to-crystalline phase ratio at about the same temperature range as determined using infrared spectrophotometry (IR). In general, the amount of the transferred PTFE on AISI 316 depended on the relative amount of amorphous phase in the PTFE contact area. Thus, the amorphous phase in semicrystalline PTFE evidently plays an active role in the transfer process.

Droplets of 1,6–di (N-carbazolyl)-2,4 hexadiyne (DCHD) polydiacetylene were prepared by room temperature evaporation of dilute (0.01 wt. %) solution of the monomer in chloroform onto amorphous carbon-coated mica substrates. High Resolution Electron Microscopy (HREM) and Selected Area Electron Diffraction (SAED) revealed small crystallographically textured droplets (∼1 μm diameter) with cracks parallel to the [001] chain direction. The droplet geometry allowed us to investigate the organization of the polymer near surfaces. It was found that the curvature of the droplet edge caused a local bending of the polymer crystal lattice. Direct imaging of the molecular structure near the droplet surface revealed that the mechanism of lattice bending was by the formation of edge dislocations. Dislocations were etched in some droplets to gain information about perturbations in structure and reactivity near the core.