Magic Angle Spinning Nuclear Magnetic Resonance (MAS-NMR) spectroscopy has been used to characterize the structural and chemical environments of B, Al, and Si in model Hanford low-activity waste glasses. The average 29Si NMR peak position was found to systematically change with changing glass composition and structure. From an understanding of the structural roles of Al and B obtained from MAS-NMR experiments, we first developed a model that reliably predicts the distribution of structural units and the average 29Si chemical shift value, δ, based purely on glass composition. A product consistency test (PCT) was used to determine the normalized elemental release (NL) from the prepared glasses. Comparison of the NMR and PCT data obtained from sodium boro-aluminosilicate glasses indicates that a rudimentary exponential relationship exists between the 29Si chemical shift value, and the boron NL value.

A wide range of ultra-fine, nano-crystalline powders and suspensions have been produced using the Rapid Thermal Decomposition of precursors in Solution (RTDS) technology. These materials include single and multi-component iron-, zirconium-, titanium-, nickel-, and chromium-oxide/oxyhydroxide powders. RTDS, which was developed at Pacific Northwest Laboratory, is a flow-through hydrothermal process capable of producing nano-crystalline particulate material at rates of up to 100 grams of solid per hour. We present the results of characterization efforts on RTDS iron oxyhydroxide and zirconium oxide systems. As-collected RTDS suspensions were characterized using optical light scattering. Separated RTDS powders were evaluated using X-ray diffraction, electron microscopy, gas adsorption analysis, thermal gravimetric analysis, and chemical analysis.

Ultra-fine, nano-crystalline six-line ferrihydrite (5Fe2O3-9H2O) and cubic zirconia (ZrÜ2) powders have been produced using the Rapid Thermal Decomposition of precursors in Solution (RTDS) technology. Nano-crystalline RTDS six-line ferrihydrite powder used as an in situ precursor for first-stage direct coal liquefaction catalysts increased the liquefied products from Blind Canyon Seam coal by 22% absolute over thermal background at 350°C. Initial sintering studies performed on nano-crystalline RTDS ZrO2 powder have also been presented and compared to predictions made from theories derived for micro-crystalline powders.

Extended x-ray absorption fine structure (EXAFS) spectroscopy has been used to determine the structural environment local to iron(III) and zirconium(IV) cations in respectively, nanoscale iron oxyhydroxide and nanoscale zirconium oxide powders. The iron oxyhydroxide powder, produced by the modified reverse micelle (MRM) technology, was found to have a short-range structure most similar to that of goethite (α-FeOOH). The short-range structure of the zirconium oxide powder, produced using the rapid thermal decomposition of solutes (RTDS) technology, was found to be a mixture of monoclinic zirconia and cubic zirconia environments.

Solution and solid state Magic Angle Spinning (MAS) Nuclear Magnetic Resonance (NMR) spectroscopy have been used to monitor the 31P signal of cyclic phosphazenes and associated linear polymers in solution and of these materials bound to alumina in stabilized dispersions. The differences between the simple solution experiments and the suspensions are being studied to determine the viability of NMR techniques to probe the chemical interactions between inorganic polymer dispersants and alumina particles. It has been observed in colloidal suspensions that the adsorption of phosphazenes onto an aluminum oxide surface causes a broadening of the 31P signal in solution NMR. This broadening is dependant on the amount of solid to polymer concentration, the amount of solids loading, the solvent polarity and the phosphazene substituent under investigation [1]. Conversely, the solid MAS experiments show a narrowing of the 31P signal upon adsorption of the phosphazene to alumina.