Publications

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A widely adopted approach to form matched seals in metals having high coefficient of thermal expansion ( CTE ), e.g. stainless steel, is the use of high CTE glass‐ceramics. With the nucleation and growth of Cristobalite as the main high‐expansion crystalline phase, the CTE of recrystallizable lithium silicate Li ₂ O–SiO ₂ –Al ₂ O ₃ –K ₂ O–B ₂ O ₃ –P ₂ O ₅ –ZnO glass‐ceramic can approach 18 ppm/°C, matching closely to the 18 ppm/°C–20 ppm/°C CTE of 304L stainless steel. However, a large volume change induced by the α‐β inversion between the low‐ and high‐ Cristobalite, a 1 ^st order displacive phase transition, results in a nonlinear step‐like change in the thermal strain of glass‐ceramics. The sudden change in the thermal strain causes a substantial transient mismatch between the glass‐ceramic and stainless steel. In this study, we developed new thermal profiles based on the SiO ₂ phase diagram to crystallize both Quartz and Cristobalite as high expansion crystalline phases in the glass‐ceramics. A key step in the thermal profile is the rapid cooling of glass‐ceramic from the peak sealing temperature to suppress crystallization of Cristobalite. The rapid cooling of the glass‐ceramic to an initial lower hold temperature is conducive to Quartz crystallization. After Quartz formation, a subsequent crystallization of Cristobalite is performed at a higher hold temperature. Quantitative X‐ray diffraction analysis of a series of quenched glass‐ceramic samples clearly revealed the sequence of crystallization in the new thermal profile. The coexistence of two significantly reduced volume changes, one at ~220°C from Cristobalite inversion and the other at ~470°C from Quartz inversion, greatly improves the linearity of the thermal strains of the glass‐ceramics, and is expected to improve the thermal strain match between glass‐ceramics and stainless steel over the sealing cycle.

High-temperature X-ray diffraction with concurrent gas chromatography (GC) was used to study cobalt disulfide cathode pellets disassembled from thermal batteries. When CoS2 cathode materials were analyzed in an air environment, oxidation of the K(Br, Cl) salt phase in the cathode led to the formation of K2SO4 that subsequently reacted with the pyrite-type CoS2 phase leading to cathode decomposition between ∼260 and 450 °C. Independent thermal analysis experiments, i.e. simultaneous thermogravimetric analysis/differential scanning calorimetry/mass spectrometry (MS), augmented the diffraction results and support the overall picture of CoS2 decomposition. Both gas analysis measurements (i.e. GC and MS) from the independent experiments confirmed the formation of SO2 off-gas species during breakdown of the CoS2. In contrast, characterization of the same cathode material under inert conditions showed the presence of CoS2 throughout the entire temperature range of analysis.

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The sequence of crystallization in a recrystallizable lithium silicate sealing glass-ceramic Li2O–SiO2–Al2O3–K2O–B2O3–P2O5–ZnO was analyzed by in situ high-temperature X-ray diffraction (HTXRD). Glass-ceramic specimens have been subjected to a two-stage heat-treatment schedule, including rapid cooling from sealing temperature to a first hold temperature 650°C, followed by heating to a second hold temperature of 810°C. Notable growth and saturation of Quartz was observed at 650°C (first hold). Cristobalite crystallized at the second hold temperature of 810°C, growing from the residual glass rather than converting from the Quartz. The coexistence of quartz and cristobalite resulted in a glass-ceramic having a near-linear thermal strain, as opposed to the highly nonlinear glass-ceramic where the cristobalite is the dominant silica crystalline phase. HTXRD was also performed to analyze the inversion and phase stability of the two types of fully crystallized glass-ceramics. While the inversion in cristobalite resembles the character of a first-order displacive phase transformation, i.e., step changes in lattice parameters and thermal hysteresis in the transition temperature, the inversion in quartz appears more diffuse and occurs over a much broader temperature range. Localized tensile stresses on quartz and possible solid-solution effects have been attributed to the transition behavior of quartz crystals embedded in the glass-ceramics.

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The structure of La2LiTaO6 has been derived from the powder X-ray powder diffraction (XRD) data. La2LiTaO6 is monoclinic with unit-cell parameters a = 5.621(1) Å, b = 5.776(1) Å, c = 7.954(2) Å, β = 90.34(2)°, space group P21/n (14), and Z = 2. The structure of La2LiTaO6 is an ordered perovskite with alternating Li and Ta octahedra. A new set of powder XRD data (d-spacing and intensity listing) has been generated to replace entry 00-039-0897 within the Powder Diffraction File. The newly elucidated structural data for La2LiTaO6 shall facilitate quantitative analysis of this impurity phase which is often observed during synthesis of the fast-ion conductor phase Li5La3Ta2O12.

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Soil accumulation on photovoltaic (PV) modules presents a challenge to long-term performance prediction and lifetime estimates due to the inherent difficulty in quantifying small changes over an extended period. Low mass loadings of soil are a common occurrence but remain difficult to quantify. In order to more accurately describe the specific effects of sparse soil films on PV systems, we have expanded upon an earlier technique to measure the optical losses due to an artificially applied obscurant film. A synthetic soil analog was sprayed onto glass coupons at very brief intervals with a high-volume, low-pressure pneumatic sprayer. Light transmission through the grime film was evaluated using a quantum efficiency test stand and UV/vis spectroscopy. A 0.1-g/m 2 grime loading was determined to be the limit of mass measurement sensitivity, which is similar to some reports of daily soil accumulation. Predictable, linear decreases in transmission were observed for samples with a mass loading between 0.1 and 0.5 g/m2. A similar change was observed for soiled coupons from an outdoor monitoring station. Collected soil from the field coupons was analyzed to develop a compositional analog for indoor studies. Natural and synthetic soils produced similar decreases in transmission.

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The monoclinic-to-tetragonal phase transition (∼70 °C) in vanadium dioxide (VO2) strongly impacts the infrared properties, which enables its use in applications such as smart window devices. Synthesis of VO 2 can be challenging due to the variability of vanadium oxide phases that may be formed. We have employed high-temperature X-ray diffraction (HTXRD) to monitor the reaction process of vanadium oxide precursor powders to form the desired tetragonal VO2 phase. Single-phase tetragonal VO2 was formed within 30 min at 420 °C in flowing N2 gas (∼50 ppm O2). The monoclinic-to-tetragonal phase transformation was observed via HTXRD at ∼70 °C with the typical ∼10 °C hysteresis (i.e. approached from above or below the transition). © International Centre for Diffraction Data 2014.

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