Publications

73 Results
Skip to search filters

14 MeV DT Neutron Test Facility at the Sandia Ion Beam Laboratory

Wampler, William R.; Doyle, Barney L.; Vizkelethy, Gyorgy V.; Bielejec, Edward S.; Snow, Clark S.; Styron, Jedediah D.; Jasica, Matthew J.

This report documents work done at the Sandia Ion Beam Laboratory to develop a capability to produce 14 Me neutrons at levels sufficient for testing radiation effects on electronic materials and components. The work was primarily enabled by a laboratory directed research and development (LDRD) project. The main elements of the work were to optimize target lifetime, test a new thin- film target design concept to reduce tritium usage, design and construct a new target chamber and beamline optimized for high-flux tests, and conduct tests of effects on electronic devices and components. These tasks were all successfully completed. The improvements in target performance and target chamber design have increased the flux and fluence of 14 MV neutrons available at the test location by several orders of magnitude. The outcome of the project is that a new capability for testing radiation-effects on electronic components from 14 MeV neutrons is now available at Sandia National Laboratories. This capability has already been extensively used for many qualification and component evaluation and development tests.

More Details
TYPE SAND Report YEAR 2019
OSTIDOI

Mechanical properties of metal dihydrides

Modelling and Simulation in Materials Science and Engineering

Schultz, Peter A.; Snow, Clark S.

First-principles calculations are used to characterize the bulk elastic properties of cubic and tetragonal phase metal dihydrides, MH2 {M = Sc, Y, Ti, Zr, Hf, lanthanides} to gain insight into the mechanical properties that govern the aging behavior of rare-earth di-tritides as the constituent 3H, tritium, decays into 3He. As tritium decays, helium is inserted in the lattice, the helium migrates and collects into bubbles, that then can ultimately create sufficient internal pressure to rupture the material. The elastic properties of the materials are needed to construct effective mesoscale models of the process of bubble growth and fracture. Dihydrides of the scandium column and most of the rareearths crystalize into a cubic phase, while dihydrides from the next column, Ti, Zr, and Hf, distort instead into the tetragonal phase, indicating incipient instabilities in the phase and potentially significant changes in elastic properties. We report the computed elastic properties of these dihydrides, and also investigate the off-stoichiometric phases as He or vacancies accumulate. As helium builds up in the cubic phase, the shear moduli greatly soften, converting to the tetragonal phase. Conversely, the tetragonal phases convert very quickly to cubic with the removal of H from the lattice, while the cubic phases show little change with removal of H. The source and magnitude of the numerical and physical uncertainties in the modeling are analyzed and quantified to establish the level of confidence that can be placed in the computational results, and this quantified confidence is used to justify using the results to augment and even supplant experimental measurements.

More Details
TYPE Journal Article YEAR 2016
ScopusOSTIDOI

In Situ Electron Microscopy of Helium Bubble Implantation in Metal Hydrides

Hattar, Khalid M.; Bufford, Daniel C.; Robinson, David R.; Snow, Clark S.

Here we investigated the microstructural response of various Pd physically vapor deposited films and Er and ErD2 samples prepared from neutron Tube targets to implanted He via in situ ion irradiation transmission electron microscopy and subsequent in situ annealing experiments. Small bubbles formed in both systems during implantation, but did not grow with increasing fluence or a short duration room temperature aging (weeks). Annealing produced large cavities with different densities in the two systems. The ErD2 showed increased cavity nucleation compared to Er. The spherical bubbles formed from high fluence implantation and rapid annealing in both Er and ErD2 cases differed from microstructures of naturally aged tritiated samples. Further work is still underway to determine the transition in bubble shape in the Er samples, as well as the mechanism for evolution in Pd films.

More Details
TYPE Other Report YEAR 2014
OSTIDOI

Characterization of the surface changes during the activation process of erbium/erbium oxide for hydrogen storage

Brumbach, Michael T.; Zavadil, Kevin R.; Snow, Clark S.; Ohlhausen, J.A.

Erbium is known to effectively load with hydrogen when held at high temperature in a hydrogen atmosphere. To make the storage of hydrogen kinetically feasible, a thermal activation step is required. Activation is a routine practice, but very little is known about the physical, chemical, and/or electronic processes that occur during Activation. This work presents in situ characterization of erbium Activation using variable energy photoelectron spectroscopy at various stages of the Activation process. Modification of the passive surface oxide plays a significant role in Activation. The chemical and electronic changes observed from core-level and valence band spectra will be discussed along with corroborating ion scattering spectroscopy measurements.

More Details
TYPE Conference YEAR 2010
OSTI

Characterization of the surface changes during the activation of erbium/erbium oxide for hydrogen storage

Zavadil, Kevin R.; Snow, Clark S.; Ohlhausen, J.A.

Erbium is known to effectively load with hydrogen when held at high temperature in a hydrogen atmosphere. To make the storage of hydrogen kinetically feasible, a thermal activation step is required. Activation is a routine practice, but very little is known about the physical, chemical, and/or electronic processes that occur during Activation. This work presents in situ characterization of erbium Activation using variable energy photoelectron spectroscopy at various stages of the Activation process. Modification of the passive surface oxide plays a significant role in Activation. The chemical and electronic changes observed from core-level and valence band spectra will be discussed along with corroborating ion scattering spectroscopy measurements.

More Details
TYPE Conference YEAR 2010
OSTI

In-situ observation of ErD2 formation during D2 loading via neutron diffraction

Rodriguez, Marko A.; Snow, Clark S.; Wixom, Ryan R.

In an effort to better understand the structural changes occurring during hydrogen loading of erbium target materials, we have performed in situ D{sub 2} loading of erbium metal (powder) at temperature (450 C) with simultaneous neutron diffraction analysis. This experiment tracked the conversion of Er metal to the {alpha} erbium deuteride (solid-solution) phase and then into the {beta} (fluorite) phase. Complete conversion to ErD{sub 2.0} was accomplished at 10 Torr D{sub 2} pressure with deuterium fully occupying the tetrahedral sites in the fluorite lattice.

More Details
TYPE Conference YEAR 2010
OSTI

Processing effects on microstructure in Er and ErD2 thin-films

Journal of Nuclear Materials

Parish, Chad M.; Snow, Clark S.; Kammler, Daniel K.; Brewer, Luke N.

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.

More Details
TYPE Journal Article YEAR 2010
ScopusOSTIDOI

Processing effects on microstructure in Er and ErD2 thin-films

Kammler, Daniel K.; Brewer, Luke N.; Snow, Clark S.

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.

More Details
TYPE Conference YEAR 2010
OSTI

The manifestation of oxygen contamination in ErD2

Proposed for publication in the International Journal of Hydrogen Energy.

Parish, Chad M.; Snow, Clark S.; Brewer, Luke N.

Erbium dihydride Er(H,D,T){sub 2} is a fluorite structure rare-earth dihydride useful for the storage of hydrogen isotopes in the solid state. However, thermodynamic predictions indicate that erbium oxide formation will proceed readily during processing, which may detrimentally contaminate Er(H,D,T){sub 2} films. In this work, transmission electron microscopy (TEM) techniques including energy-dispersive x-ray spectroscopy, energy-filtered TEM, selected area electron diffraction, and high-resolution TEM are used to examine the manifestation of oxygen contamination in ErD{sub 2} thin films. An oxide layer {approx}30-130 nm thick was found on top of the underlying ErD{sub 2} film, and showed a cube-on-cube epitaxial orientation to the underlying ErD{sub 2}. Electron diffraction confirmed the oxide layer to be Er{sub 2}O{sub 3}. While the majority of the film was observed to have the expected fluorite structure for ErD{sub 2}, secondary diffraction spots suggested the possibility of either nanoscale oxide inclusions or hydrogen ordering. In situ heating experiments combined with electron diffraction ruled out the possibility of hydrogen ordering, so epitaxial oxide nanoinclusions within the ErD{sub 2} matrix are hypothesized. TEM techniques were applied to examine this oxide nanoinclusion hypothesis.

More Details
TYPE Journal Article YEAR 2008
OSTI

In-situ time-of-flight neutron diffraction of ErD2 (beta phase) formation during D2 loading

Rodriguez, Marko A.; Snow, Clark S.; Wixom, Ryan R.

In an effort to better understand the structural changes occurring during hydrogen loading of erbium target materials, we have performed D{sub 2} loading of erbium metal (powder) with simultaneous neutron diffraction analysis. This experiment tracked the conversion of Er metal to the {alpha} erbium deuteride (solid-solution) phase and then on to the {beta} (fluorite) phase. Complete conversion to ErD{sub 2.0} was accomplished at 10 Torr D{sub 2} pressure with deuterium fully occupying the tetrahedral sites in the fluorite lattice. Increased D{sub 2} pressure (up to 500 Torr at 450 C) revealed {approx}10 % deuterium occupation of the octahedral sites. Subsequent vacuum pumping of the sample at 450 C removed octahedral site occupancy while maintaining tetrahedral deuterium occupancy, thereby yielding stoichiometric ErD{sub 2.0} {beta} phase.

More Details
TYPE SAND Report YEAR 2008
OSTIDOI

Summary of Sandia research on metal tritides : FY 2007

Snow, Clark S.; Kammler, Daniel K.; Ferrizz, Robert F.; Espada Castillo, Loren I.; Wixom, Ryan R.; Rodriguez, Marko A.

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.

More Details
TYPE SAND Report YEAR 2008
OSTIDOI

Helium release and microstructural changes in Er(D,T)2-x3Hex films)

Snow, Clark S.; Brewer, Luke N.; Rodriguez, Marko A.; Kotula, Paul G.; Banks, J.C.; Mangan, Michael M.

Er(D,T){sub 2-x} {sup 3}He{sub x}, erbium di-tritide, films of thicknesses 500 nm, 400 nm, 300 nm, 200 nm, and 100 nm were grown and analyzed by Transmission Electron Microscopy, X-Ray Diffraction, and Ion Beam Analysis to determine variations in film microstructure as a function of film thickness and age, due to the time-dependent build-up of {sup 3}He in the film from the radioactive decay of tritium. Several interesting features were observed: One, the amount of helium released as a function of film thickness is relatively constant. This suggests that the helium is being released only from the near surface region and that the helium is not diffusing to the surface from the bulk of the film. Two, lenticular helium bubbles are observed as a result of the radioactive decay of tritium into {sup 3}He. These bubbles grow along the [111] crystallographic direction. Three, a helium bubble free zone, or 'denuded zone' is observed near the surface. The size of this region is independent of film thickness. Four, an analysis of secondary diffraction spots in the Transmission Electron Microscopy study indicate that small erbium oxide precipitates, 5-10 nm in size, exist throughout the film. Further, all of the films had large erbium oxide inclusions, in many cases these inclusions span the depth of the film.

More Details
TYPE SAND Report YEAR 2007
OSTIDOI
73 Results
73 Results