Publications

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Thermogravimetric analysis - gas chromatography/mass spectrometry (TGA- GC/MS) experiments were performed on EN-7 and EN-8, analyzed, and reported in [1] . This SAND report derives and describes pyrolytic thermal decomposition models for use in predicting the responses of EN-7 and EN-8 in an abnormal thermal environment.

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Here we are investigating the inclusion of organotin compounds in polystyrene material to improve plastic scintillators full gamma-ray energy sensitivity with the ultimate goal of achieving spectroscopy. Accurate evaluation of the relative light yield from the newly developed scintillators is crucial to assess merits of compounds and chemical processes used in the scintillators development and assess the scintillation efficiencies of the newly produced scintillators. Full gamma-ray energy peak in the measured gamma-ray spectrum, resulting from total absorption of gamma-ray energy, would be ideal in assessing the relative light yield. However, the significant number of new samples we are producing for investigation lead us to the possibility of using the Compton edge as an alternate spectral feature that can be exploited for expeditious characterization of the relative light yield in plastic scintillators. In this study we present a spectra gain matching approach, using a spectrum rebinning, for accurate relative light yield measurement using the Compton edge.

The thermal degradation of two polyurethane elastomers was investigated via thermal gravimetric analysis coupled with gas chromatography/ma ss spectrometry. Decomposition occur s in a multi - step fashion with similar onset temperatures for both materials. Apparent activation energy plots were calculated inside Model - Free Kinetics software and utilized to construct conversion and isothermal conversion tables . These tables predicted material degradation as a function of temperature and time. Isothermal experiments were performed and found to be in good agreement with the predictions made from the Model - Free Kinetic s software package. Volatile products evolved during the multistep decomposition were captured at various times and analyzed using the coupled gas chromatography/mass spectrometry system . This analysis demonstrated strong correlation between the degradation products and known decomposition mechanisms for polyurethanes.

Melt state dynamics for a series of strictly linear polyethylenes with precisely spaced associating functional groups were investigated. The periodic pendant acrylic acid groups form hydrogen-bonded acid aggregates within the polyethylene (PE) matrix. The dynamics of these nanoscale heterogeneous morphologies were investigated from picosecond to nanosecond timescales by both quasi-elastic neutron scattering (QENS) measurements and fully atomistic molecular dynamics (MD) simulations. Two dynamic processes were observed. The faster dynamic processes which occur at the picosecond timescales are compositionally insensitive and indicative of spatially restricted local motions. The slower dynamic processes are highly composition dependent and indicate the structural relaxation of the polymer backbone. Higher acid contents, or shorter PE spacers between pendant acid groups, slow the structural relaxation timescale and increase the stretching parameter (β) of the structural relaxation. Additionally, the dynamics of specific hydrogen atom positions along the backbone correlate structural heterogeneity imposed by the associating acid groups with a mobility gradient along the polymer backbone. At time intervals (<2 ns), the mean-squared displacements for the four methylene groups closest to the acid groups are up to 10 times smaller than those of methylene groups further from the acid groups. At longer timescales acid aggregates rearrange and the chain dynamics of the slow, near-aggregate regions and the faster bridge regions converge, implying a characteristic timescale for the passage of chains between aggregates. The characterization of the nanoscale chain dynamics in these associating polymer systems both provides validation of simulation force fields and provides understanding of heterogeneous chain dynamics in associating polymers.

Decomposition profiles for individual and mixed foam samples were examined in partially confined and unconfined environments. The weight percent loss versus temperature plots for the individual and mixed foams show that foams in a partially confined environment experience decomposition at a higher onset temperature than do foams in an unconfined environment. Likewise, the decomposition profiles of foams and mixed foams in a partially con fined environment differed from the decomposition profiles of these materials in an unconfined environment. These results suggest that different environments affect the decomposition mechanisms of foams. Furthermore, derivative thermogravimetric analysis showed that mixed foam samples decompose differently than do their individual parts, indicating that a foam will undergo a different mechanism of decomposition when heated in the presence of other foams than when heated alone.

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The insulation resistance (R_I) between parallel copper traces embedded on flexible, polyimide-based circuit boards was measured as a function of temperature, substrate type, copper thickness, and feature size. The results show a strong dependency on temperature: the measured R_I decreases nearly seven-orders of magnitude upon a 90degC change. Also measured was R_I as a function of the trace and space of parallel copper circuits. This dependency is less obvious but a correlation showing narrower spacing leads to lower R_I is evident. The thickness/width of the copper traces has less of an effect on the measured R_I. The thickness of the polyimide-based substrate, or core of the circuit boards, was also varied. Measurements of the R_I versus substrate thickness were inconclusive. The height of the copper traces was changed and shows that heavier (or taller traces) result in a lower measured R_I. Lastly, it was shown that the adhesive found between the copper traces and the polyimide core on so-called "LF" Pyralux^(R) boards significantly reduces the measured R_I compared to "AP" Pyralux^(R) boards of the same dimensions. The presences of this adhesive in all LF materials, including LF coverlays should be avoided if high R_I is desired for narrowly spaced copper traces. Alternative materials like AP Pyralux^(R) or HT Pyralux^(R) available from DuPont^TM should be investigated when designing copper-based flat-flex circuit boards that require a demanding environmental specifications.

In this work, we report the synthesis and inclusion of rationally designed organotin compounds in polystyrene matrices as a route towards plastic scintillators capable of gamma-ray spectroscopy. Tin loading ratios of up to 15% w/w have been incorporated, resulting in photopeak energy resolution values as low as 10.9% for 662 keV gamma-rays. Scintillator constituents were selected based upon a previously reported distance-dependent quenching mechanism. Data obtained using UV-Vis and photoluminescence measurements are consistent with this phenomenon and are correlated with the steric and electronic properties of the respective organotin complexes. We also report fast scintillation decay behavior that is comparable to the quenched scintillators 0.5% trans-stilbene doped bibenzyl and the commercial plastic scintillator BC-422Q-1%. These observations are discussed in the context of practical considerations such as optical transparency, ease-of-preparation/scale-up, and total scintillator cost.

Currently we are investigating the inclusion of organotin compounds in polystyrene material to improve plastic scintillators full gamma-ray energy sensitivity with the ultimate goal of achieving spectroscopy. Accurate evaluation of light yield from the newly developed scintillators is crucial to assess merits of compounds and chemical process used in the scintillators development. Full gamma-ray energy peak in measured gammaray spectrum, resulting from total absorption of gamma-ray energy, would be ideal in evaluating the light yield from the new scintillators. However, full energy sensitivity achieved thus far is not statistically viable for fast and accurate light yield energy calibration from the new scintillators. The Compton edge in measured gamma-ray spectrum has been found as an alternate gamma-ray spectrum feature that can be exploited for characterizing the light yield energy from the newly developed plastic scintillators. In this study we present technique implemented for accurate light yield energy calibration using the Compton edge. Results obtained were very encouraging and promise the possibility of using the Compton edge for energy calibration in detectors with poor energy resolution such as plastic and liquid scintillators.

Two types of water - containing liquid scintillation mixtures were prepared in the present work. In the first, m ixtures of 2 - phenylethanol, water, diphenyl phosphate, sodium phenyl phosphate dibasic dihydrate, and the dye 2,5 - diphenyloxazole (PPO) have been investigated as liquid scintillators. In the second system, nonionic and mixed surfactant systems were investigated in conjunction with water and small amounts of toluene. In both cases, increasing amounts of water led to reductions in the scintillation light yield. Understanding what factors contr ibute to this phenomenon is the focus of this report. Changes in the solution microphase structure, diminishing aromatic content of the cocktail mixtures, and inefficient energy transfer to the dye a ppear to be responsible for the decreased light yield as more water is added . In the 2 - phenylethanol system, the observed experimental results are consistent with the formation of a bicontinuous microemulsion at higher water concentrations, which incorporates PPO and shields it from the quenching effects of the increasing polar matrix. Evidence for this proposed phase change comes from light scattering data, photo - and x - ray luminescence measurements, and optical transparency measurements . In the surfactant - based system, the quenching effect of water was found to be less than both commercially - available dioxane - naphthalene mixtures used for scintillation counting as well as the 2 - phenylethanol mixtures described above. The effect of different surfactant mixtures and concentrations were studied, revealing a benefic ial effect upon the scintillation light yield for mixed surfactant mixtures. These results are interpreted in the context of reactive radical species formation following water ionization , which leads to light - yield quenching in aqueous systems . The presence of surfactant(s) in these mixtures enables the formation of organic - rich regions that are spatially separated from the reactive radicals. This hypothesis is consistent with subsequent experiments that showed reduced light - yield quenching in the presence of radical - trapping additives. A notable result from these surfactant studies was the preparation of an aqueous scintillator that was transparent and showed neutron/gamma pulse - shape discrimination. Section II below provides background information on the significance of this finding. The combined work described herein has implications on other efforts to make water - based solution scintillators -- without aromatic content an efficient mechanism for ionizing radiation to sensitize emission from a dye is limited.

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Synthesis of ditopic imidazoliums was achieved using a modular step-wise procedure. The procedure itself is amenable to a wide array of functional groups that can be incorporated into the imidazolium architecture. The resulting compounds range from ditopic zwitterions to highly-soluble dicationic aromatics

In this report we explore the sensitivities of the insulation resistance between two loops of wire embedded in insulating materials with a simple, approximate model. We discuss limita- tions of the model and ideas for improvements.

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