Increased interest in ceramic materials, particularly for high-temperature, high-stress applications, has created the need for rapid and reliable analytical techniques to monitor microcrystalline structure of commercial ceramic powders. A comparative evaluation of commercially available PSiC powders is undertaken to analyze the potential of nuclear magnetic resonance (NMR) in the characterization of PSiC powder. NMR provides an acceptable, rapid method for characterization of powders both during powder manufacturing as well as for powder analyses prior to sintering studies. The results of transmission electron microscopy and X-ray diffraction are correlated with the NMR spectra to explain some newly observed features in the NMR spectra of PSiC powders and to illustrate the sensitivity of NMR to microcrystalline disorder. [Key words: microscopy, nuclear magnetic resonance, transmission electron microscopy, X-ray diffraction, silicon carbide.]
Polyester blends may undergo transesterification during processing, resulting in molecular rearrangements, transient properties, and eventually, degradation. To suppress transesterifcation, the use of organophosphites has been suggested in the patent and technical literature. The effectiveness of organophosphites, however, is variable and sometimes inconsistent. Our recent studies suggest a clue to the inconsistent behavior and provide a simple way to enhance the effectiveness of these stabilizers. Using solid state 31P NMR it was shown that for bis(2,4-di-t-butylphenyl)pentaerythritol diphosphite a conversion of the phosphite group to a phosphonate, via hydrolysis, is a prerequisite for a n effective inhibition of transesterification. This conversion occurs readily during melt compounding if the polymers are not completely dry. However, if rigorous drying is employed and phosphite conversion does not occur, then transesterification is not arrested. It was also found that over a period of time the conversion of the phosphite to a phosphonate may take place at room temperature as well. After aging for about a year in the laboratory, the originally ineffective compound, has become a very effective inhibitor of transesterification in blends containing poly(ethy1ene terephthalate), poly(buty1ene terephthalate), polycarbonate, and polyarylate. Thus, a simple way to enhance the phosphite effectiveness is to expose it to a humid environment prior to blending.
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