Publications

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Erbium metal thin-films have been deposited on molybdenum-on-silicon substrates and then converted to erbium dideuteride (ErD2). Here, we study the effects of deposition temperature (≈300 or 723 K) and deposition rate (1 or 20 nm/s) upon the initial Er metal microstructure and subsequent ErD2 microstructure. We find that low deposition temperature and low deposition rate lead to small Er metal grain sizes, and high deposition temperature and deposition rate led to larger Er metal grain sizes, consistent with published models of metal thin-film growth. ErD2 grain sizes are strongly influenced by the prior-metal grain size, with small metal grains leading to large ErD2 grains. A novel sample preparation technique for electron backscatter diffraction of air-sensitive ErD2 was developed, and allowed the quantitative measurement of ErD2 grain size and crystallographic texture. Finer-grained ErD2 showed a strong (1 1 1) fiber texture, whereas larger grained ErD2 had only weak texture. We hypothesize that this inverse correlation may arise from improved hydrogen diffusion kinetics in the more defective fine-grained metal structure or due to improved nucleation in the textured large-grain Er. © 2010 Elsevier B.V. All rights reserved.

Erbium metal thin-films have been deposited on molybdenum-on-silicon substrates and then converted to erbium dideuteride (ErD{sub 2}). Here, we study the effects of deposition temperature ({approx}300 or 723 K) and deposition rate (1 or 20 nm/s) upon the initial Er metal microstructure and subsequent ErD{sub 2} microstructure. We find that low deposition temperature and low deposition rate lead to small Er metal grain sizes, and high deposition temperature and deposition rate led to larger Er metal grain sizes, consistent with published models of metal thin-film growth. ErD{sub 2} grain sizes are strongly influenced by the prior-metal grain size, with small metal grains leading to large ErD{sub 2} grains. A novel sample preparation technique for electron backscatter diffraction of air-sensitive ErD{sub 2} was developed, and allowed the quantitative measurement of ErD{sub 2} grain size and crystallographic texture. Finer-grained ErD{sub 2} showed a strong (1 1 1) fiber texture, whereas larger grained ErD{sub 2} had only weak texture. We hypothesize that this inverse correlation may arise from improved hydrogen diffusion kinetics in the more defective fine-grained metal structure or due to improved nucleation in the textured large-grain Er.

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The mechanisms governing D loss in ErD2 films with and without a Mo diffusion barrier on kovar substrates were studied between 200 and 600 °C via in-situ Ion Beam Analysis (IBA). Significant intermixing between kovar and Er was observed above 450°C and between kovar and ErD2 above 500 °C. The D loss mechanism in ErD2 films was found to change from intermixing between kovar and ErD2 at low temperatures (< 500 °C) to thermal decomposition at higher temperatures (> 500 °C). Diffusion between kovar and ErD2 was measured isothermally at 500 and 550 °C. An activation energy of 2.1 eV and a pre-exponential factor of 0.071 cm2/s were determined. Diffusion between the kovar components and ErD2 film was inhibited by depositing a 200 nm Mo diffusion barrier between the kovar substrate and the ErD2 film. The processing of the Mo diffusion barrier was shown to impact its performance. Intermixing between the kovar / Mo / ErD2 stack becomes significant between 500 and 550 °C with a sputter deposited Mo diffusion barrier and between 550 and 600 °C for an electron-beam evaporated Mo diffusion barrier. Copyright © 2009 ASM International® All rights reserved.

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{sm_bullet}Mixing from some thermal process steps thought to drive H,D,T loss - This does not appear to be a problem with the Mo/Er occluder stacks {sm_bullet}Diffusion barriers investigated to prevent mixing

Sandia National Laboratories has cradle to grave responsibility for all neutron generators in the US nuclear weapons stockpile. As such, much research effort is exerted to develop a comprehensive understanding of all the major components of a neutron generator. One of the key components is the tritium containing target. The target is a thin metal tritide film. Sandia's research into metal tritides began in the early 1960's with a collaboration with the Denver Research Institute (DRI) and continues to this day with a major in house research effort. This document is an attempt to briefly summarize what is known about the aging of erbium tritide and to review the major publications conducted at Sandia in FY 07. First, a review of our knowledge of helium in erbium tritide will be presented. Second, executive summaries of the six major SAND reports regarding neutron tube targets published in FY07 by Department 2735, the Applied Science and Technology Maturation Department, and research partners are presented.

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The potential for electrochromic (EC) materials to be incorporated into a Fabry-Perot (FP) filter to allow modest amounts of tuning was evaluated by both experimental methods and modeling. A combination of chemical vapor deposition (CVD), physical vapor deposition (PVD), and electrochemical methods was used to produce an ECFP film stack consisting of an EC WO{sub 3}/Ta{sub 2}O{sub 5}/NiO{sub x}H{sub y} film stack (with indium-tin-oxide electrodes) sandwiched between two Si{sub 3}N{sub 4}/SiO{sub 2} dielectric reflector stacks. A process to produce a NiO{sub x}H{sub y} charge storage layer that freed the EC stack from dependence on atmospheric humidity and allowed construction of this complex EC-FP stack was developed. The refractive index (n) and extinction coefficient (k) for each layer in the EC-FP film stack was measured between 300 and 1700 nm. A prototype EC-FP filter was produced that had a transmission at 500 nm of 36%, and a FWHM of 10 nm. A general modeling approach that takes into account the desired pass band location, pass band width, required transmission and EC optical constants in order to estimate the maximum tuning from an EC-FP filter was developed. Modeling shows that minor thickness changes in the prototype stack developed in this project should yield a filter with a transmission at 600 nm of 33% and a FWHM of 9.6 nm, which could be tuned to 598 nm with a FWHM of 12.1 nm and a transmission of 16%. Additional modeling shows that if the EC WO{sub 3} absorption centers were optimized, then a shift from 600 nm to 598 nm could be made with a FWHM of 11.3 nm and a transmission of 20%. If (at 600 nm) the FWHM is decreased to 1 nm and transmission maintained at a reasonable level (e.g. 30%), only fractions of a nm of tuning would be possible with the film stack considered in this study. These tradeoffs may improve at other wavelengths or with EC materials different than those considered here. Finally, based on our limited investigation and material set, the severe absorption associated with the refractive index change suggests that incorporating EC materials into phase correcting spatial light modulators (SLMS) would allow for only negligible phase correction before transmission losses became too severe. However, we would like to emphasize that other EC materials may allow sufficient phase correction with limited absorption, which could make this approach attractive.

Electrochromic (EC) materials are used in 'smart' windows that can be darkened by applying a voltage across an EC stack on the window. The associated change in refractive index (n) in the EC materials might allow their use in tunable or temperature-insensitive Fabry-Perot filters and transmissive-spatial-light-modulators (SLMs). The authors are conducting a preliminary evaluation of these materials in many applications, including target-in-the-loop systems. Data on tungsten oxide, WO{sub 3}, the workhorse EC material, indicate that it's possible to achieve modest changes in n with only slight increases in absorption between the visible and {approx}10 {micro}m. This might enable construction of a tunable Fabry-Perot filter consisting of an active EC layer (e.g. WO{sub 3}) and a proton conductor (e.g.Ta{sub 2}O{sub 5}) sandwiched between two gold electrodes. A SLM might be produced by replacing the gold with a transparent conductor (e.g. ITO). This SLM would allow broad-band operation like a micromirror array. Since it's a transmission element, simple optical designs like those in liquid-crystal systems would be possible. Our team has fabricated EC stacks and characterized their switching speed and optical properties (n, k). We plan to study the interplay between process parameters, film properties, and performance characteristics associated with the FP-filter and then extend what we learn to SLMs. Our goals are to understand whether the changes in absorption associated with changes in n are acceptable, and whether it's possible to design an EC-stack that's fast enough to be interesting. We'll present our preliminary findings regarding the potential viability of EC materials for target-in-the-loop applications.

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