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Airborne contaminants from fires containing nuclear waste represent significant health hazards and shape the design and operation of nuclear facilities. Much of the data used to formulate DOE-HDBK-3010-94, "Airborne Release Fractions/Rates and Respirable Fractions for Nonreactor Nuclear Facilities," from the U.S. Department of Energy, were taken over 40 years ago. The objectives of this study were to reproduce experiments from Pacific Northwest Laboratories conducted in June 1973 employing current aerosol measurement methods and instrumentation, develop an enhanced understanding of particulate formation and transport from fires containing nuclear waste, and provide modeling and experimental capabilities for updating current standards and practices in nuclear facilities. A special chamber was designed to conduct small fires containing 25 mL of flammable waste containing lutetium nitrate, ytterbium nitrate, or depleted uranium nitrate. Carbon soot aerosols showed aggregates of primary particles ranging from 20 to 60 nm in diameter. In scanning electron microscopy, ~200-nm spheroidal particles were also observed dispersed among the fractal aggregates. The 200-nm spherical particles were composed of metal phosphates. Airborne release fractions (ARFs) were characterized by leaching filter deposits and quantifying metal concentrations with mass spectrometry. The average mass-based ARF for 238U experiments was 1.0 × 10−3 with a standard deviation of 7.5 × 10−4. For the original experiments, DOE-HDBK-3010-94 states, "Uranium ARFs range from 2 × 10−4 to 3 × 10−3, an uncertainty of approximately an order of magnitude." Thus, current measurements were consistent with DOE-HDBK-3010-94 values. ARF values for lutetium and ytterbium were approximately one to two orders of magnitude lower than 238U. Metal nitrate solubility may have varied with elemental composition and temperature, thereby affecting ARF values for uranium surrogates (Yb and Lu). In addition to ARF data, solution boiling temperatures and evaporation rates can also be deduced from experimental data. [ABSTRACT FROM AUTHOR]

Solution deposition is widely used for the fabrication of lead zirconate titanate (PZT) thin films on platinized silicon substrates. However, phase and texture evolution during the crystallization process is not well understood, particularly due to the difficulty in tracking changes in the thin films in situ during heating. In this work, we characterized phase and texture evolution in situ during heating and crystallization of PZT thin films using high-energy X-ray diffraction. Films were pyrolyzed at either 300 °C or 400 °C and heated at various rates between 0.5 °C/s and ∼150 °C/s. For films that were pyrolyzed at 300 °C, the most rapid heating rates first induced strong intensities from a transient Pt3Pb phase. The Pt3Pb phase inherited the texture of the pre-existing platinum layer. Combined with other observations, the results suggest the conversion of the platinum to the intermetallic phase near the interface due to the interdiffusion of lead. In all experimental variations, the pyrochlore phase was observed to form concurrently with the disappearance of the Pt3Pb phase after which the perovskite phase ultimately crystallized. For films that were pyrolyzed at 400 °C, the Pt3Pb phase was not observed at any of the heating rates; instead, the pyrochlore phase was first observed, followed by the perovskite phase. Independent of the pyrolysis temperature or observation of Pt3Pb, a 111-dominant crystallographic texture formed in the perovskite phase when crystallized using fast heating rates. These results demonstrate that 111 textures in solution-derived PZT thin films are not correlated with the observation of Pt3Pb or other intermetallic or transient phases. [ABSTRACT FROM AUTHOR]

Many microsystems fabrication technologies currently employ a metallic overlayer, such as gold, in electrical contact with silicon structural layers. During postprocessing in hydrofluoric-based acid solutions, a galvanic cell is created between the silicon and the metallic layer. Micromachined tensile specimens reveal that such etching in the presence of a galvanic cell can cause a catastrophic reduction in the tensile strength and apparent modulus of silicon. Detailed failure analysis was also used to compare fractured corroded Si to otherwise identical reference specimens via surface based (electron and scanning probe) microscopy as well as cross-section based structural- and composition-characterization techniques. For both polycrystalline and single-crystal silicon, galvanic corrosion can result in a thick corroded surface layer created via porous silicon formation, and/or generalized material removal depending on the etch chemistry and conditions. Under certain etching conditions, the porous silicon formation process results in cavity formation as well as preferential grain-boundary attack leading to intergranular fracture. The nature and severity of corrosion damage are shown to be influenced by the surface wetting characteristics of the etch chemistry, with poor wetting resulting in localized attack facilitated by the microstructure and good wetting resulting in generalized attack. The measured stiffness of the tensile specimens can be used to determine the effective modulus and porosity of the corroded surface layer. Extending beyond previous investigations, the present work examines the quantitative connection between the choice of chemical etchant, the corresponding damage morphology, and the resulting degradation in strength and apparent modulus. The present work also uniquely identifies important differences in polycrystalline and single-crystal Si based on their disparate damage evolution and related mechanical performance. [ABSTRACT FROM AUTHOR]