Publications

Abstract not provided.

Aluminum oxide (ALOX) filled epoxy is the dielectric encapsulant in shock driven high-voltage power supplies. ALOX encapsulants display a high dielectric strength under purely electrical stress, but minimal information is available on the combined effects of high voltage and mechanical shock. We report breakdown results from applying electrical stress in the form of a unipolar high-voltage pulse of the order of 10-{micro}s duration, and our findings may establish a basis for understanding the results from proposed combined-stress experiments. A test specimen geometry giving approximately uniform fields is used to compare three ALOX encapsulant formulations, which include the new-baseline 459 epoxy resin encapsulant and a variant in which the Alcoa T-64 alumina filler is replaced with Sumitomo AA-10 alumina. None of these encapsulants show a sensitivity to ionizing radiation. We also report results from specimens with sharp-edged electrodes that cause strong, localized field enhancement as might be present near electrically-discharged mechanical fractures in an encapsulant. Under these conditions the 459-epoxy ALOX encapsulant displays approximately 40% lower dielectric strength than the older Z-cured Epon 828 formulation. An investigation of several processing variables did not reveal an explanation for this reduced performance. The 459-epoxy encapsulant appears to suffer electrical breakdown if the peak field anywhere reaches a critical level. The stress-strain characteristics of Z-cured ALOX encapsulant are measured under high triaxial pressure and we find that this stress causes permanent deformation and a network of microscopic fractures. Recommendations are made for future experimental work.

The goal of this work is to develop techniques for measuring gradients in particle concentration within filled polymers, such as encapsulant. A high concentration of filler particles is added to such materials to tailor physical properties such as thermal expansion coefficient. Sedimentation and flow-induced migration of particles can produce concentration gradients that are most severe near material boundaries. Therefore, techniques for measuring local particle concentration should be accurate near boundaries. Particle gradients in an alumina-filled epoxy resin are measured with a spatial resolution of 0.2 mm using an x-ray beam attenuation technique, but an artifact related to the finite diameter of the beam reduces accuracy near the specimen's edge. Local particle concentration near an edge can be measured more reliably using microscopy coupled with image analysis. This is illustrated by measuring concentration profiles of glass particles having 40 {micro}m median diameter using images acquired by a confocal laser fluorescence microscope. The mean of the measured profiles of volume fraction agrees to better than 3% with the expected value, and the shape of the profiles agrees qualitatively with simple theory for sedimentation of monodisperse particles. Extending this microscopy technique to smaller, micron-scale filler particles used in encapsulant for microelectronic devices is illustrated by measuring the local concentration of an epoxy resin containing 0.41 volume fraction of silica.

This report documents an improved preparation of low density microcellular carbon as well as characterization of spatial homogeneity. The report also documents the process for preparing the nficrocellular carbon from poly(acrylonitrile) raw material. A microcellular polymer precursor (0.025 g/cc) is first prepared via a solution-based process and then pyrolyzed to produce the microcellular carbon in a monolithic form (0.05 g/cc). The process improvement developed in this study permits the pore structure of the n-ficrocellular polymer precursor and the microcellular carbon to be reproduced consistently in different laboratories. Pore structure is affected by the completeness of dissolution of the polymer raw material, which variable can be adjusted via dissolution temperature or particle size of the raw material. The second topic in this report involves determining the spatial fluctuation in mass density caused by periodic, millimeter-scale bands, known as `tree rings` visible on machined surfaces of the carbon monoliths. To measure the fluctuations, we developed a high precision, spatially resolved X-ray transmission technique. The periodic bands caused less than {plus_minus}2% variation of mass density in a microcellular carbon having average density 0.041 g/cc.

This work concerns preparing tailored porous carbon monoliths by pyrolyzing porous polymer precursors. Prior work in this laboratory (1) demonstrated that a low density (0.05 g/cm{sup 3}), high void fraction (97 vol%) carbon monolith could be prepared by pyrolyzing a porous poly(acrylonitrile) (PAN) precursor. A higher density, more robust carbon material is preferred for certain applications, such as electrodes for electrochemical devices. The present work demonstrates that porous carbon monoliths having mass density of 0.7 g/cm{sup 3} can be prepared from a porous PAN precursor if the pyrolysis is controlled carefully. The macropore structure of the carbon is adjusted by changing the pore structure of the PAN precursor, and the finer scale structure (such as the crystallite size L{sub c}) is adjusted by varying the pyrolysis or heat treatment temperature.

Microporous polymers are useful for applications as diverse as separation membranes and physical supports for chemically active species. One of the most important preparation methods employs thermal demixing of solution. Differences in the morphology of thermally demixed 2 wt% solutions of PAN in maleic anhydride cannot be explained by existing models, which are based on phase diagrams. An explanation based on degradation of the polymer is not supported by GPC, NMR, or FTIR experiments. We speculate that the physical structure of the polymer in solution, involving either intramolecular dimensions or intermolecular aggregation, has an important effect on the morphology.