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Title: Investigating Helium Bubble Nucleation and Growth through Simultaneous In-Situ Cryogenic, Ion Implantation, and Environmental Transmission Electron Microscopy

Abstract

Palladium can readily dissociate molecular hydrogen at its surface, and rapidly accept it onto the octahedral sites of its face-centered cubic crystal structure. This can include radioactive tritium. As tritium β-decays with a half-life of 12.3 years, He-3 is generated in the metal lattice, causing significant degradation of the material. Helium bubble evolution at high concentrations can result in blister formation or exfoliation and must therefore be well understood to predict the longevity of materials that absorb tritium. A hydrogen over-pressure must be applied to palladium hydride to prevent hydrogen from desorbing from the metal, making it difficult to study tritium in palladium by methods that involve vacuum, such as electron microscopy. Recent improvements in in-situ ion implantation Transmission Electron Microscopy (TEM) allow for the direct observation of He bubble nucleation and growth in materials. In this work, we present results from preliminary experiments using the new ion implantation Environmental TEM (ETEM) at the University of Huddersfield to observe He bubble nucleation and growth, in-situ, in palladium at cryogenic temperatures in a hydrogen environment. After the initial nucleation phase, bubble diameter remained constant throughout the implantation, but bubble density increased with implantation time. β-phase palladium hydride was not observed tomore » form during the experiments, likely indicating that the cryogenic implantation temperature played a dominating role in the bubble nucleation and growth behavior.« less

Authors:
 [1]; ORCiD logo [2];  [3];  [1];  [3];  [1];  [1]; ORCiD logo [1];  [3]
  1. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
  2. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States) ; Oregon State Univ., Corvallis, OR (United States)
  3. Univ. of Huddersfield (United Kingdom)
Publication Date:
Research Org.:
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org.:
USDOE National Nuclear Security Administration (NNSA)
OSTI Identifier:
1628410
Grant/Contract Number:  
NA0003525
Resource Type:
Accepted Manuscript
Journal Name:
Materials
Additional Journal Information:
Journal Volume: 12; Journal Issue: 16; Journal ID: ISSN 1996-1944
Publisher:
MDPI
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; Materials Science; in-situ; helium implantation; environmental transmission electron microscopy; palladium tritide

Citation Formats

Taylor, Caitlin A., Briggs, Samuel, Greaves, Graeme, Monterrosa, Anthony, Aradi, Emily, Sugar, Joshua D., Robinson, David B., Hattar, Khalid, and Hinks, Jonathan A. Investigating Helium Bubble Nucleation and Growth through Simultaneous In-Situ Cryogenic, Ion Implantation, and Environmental Transmission Electron Microscopy. United States: N. p., 2019. Web. https://doi.org/10.3390/ma12162618.
Taylor, Caitlin A., Briggs, Samuel, Greaves, Graeme, Monterrosa, Anthony, Aradi, Emily, Sugar, Joshua D., Robinson, David B., Hattar, Khalid, & Hinks, Jonathan A. Investigating Helium Bubble Nucleation and Growth through Simultaneous In-Situ Cryogenic, Ion Implantation, and Environmental Transmission Electron Microscopy. United States. https://doi.org/10.3390/ma12162618
Taylor, Caitlin A., Briggs, Samuel, Greaves, Graeme, Monterrosa, Anthony, Aradi, Emily, Sugar, Joshua D., Robinson, David B., Hattar, Khalid, and Hinks, Jonathan A. Thu . "Investigating Helium Bubble Nucleation and Growth through Simultaneous In-Situ Cryogenic, Ion Implantation, and Environmental Transmission Electron Microscopy". United States. https://doi.org/10.3390/ma12162618. https://www.osti.gov/servlets/purl/1628410.
@article{osti_1628410,
title = {Investigating Helium Bubble Nucleation and Growth through Simultaneous In-Situ Cryogenic, Ion Implantation, and Environmental Transmission Electron Microscopy},
author = {Taylor, Caitlin A. and Briggs, Samuel and Greaves, Graeme and Monterrosa, Anthony and Aradi, Emily and Sugar, Joshua D. and Robinson, David B. and Hattar, Khalid and Hinks, Jonathan A.},
abstractNote = {Palladium can readily dissociate molecular hydrogen at its surface, and rapidly accept it onto the octahedral sites of its face-centered cubic crystal structure. This can include radioactive tritium. As tritium β-decays with a half-life of 12.3 years, He-3 is generated in the metal lattice, causing significant degradation of the material. Helium bubble evolution at high concentrations can result in blister formation or exfoliation and must therefore be well understood to predict the longevity of materials that absorb tritium. A hydrogen over-pressure must be applied to palladium hydride to prevent hydrogen from desorbing from the metal, making it difficult to study tritium in palladium by methods that involve vacuum, such as electron microscopy. Recent improvements in in-situ ion implantation Transmission Electron Microscopy (TEM) allow for the direct observation of He bubble nucleation and growth in materials. In this work, we present results from preliminary experiments using the new ion implantation Environmental TEM (ETEM) at the University of Huddersfield to observe He bubble nucleation and growth, in-situ, in palladium at cryogenic temperatures in a hydrogen environment. After the initial nucleation phase, bubble diameter remained constant throughout the implantation, but bubble density increased with implantation time. β-phase palladium hydride was not observed to form during the experiments, likely indicating that the cryogenic implantation temperature played a dominating role in the bubble nucleation and growth behavior.},
doi = {10.3390/ma12162618},
journal = {Materials},
number = 16,
volume = 12,
place = {United States},
year = {2019},
month = {8}
}

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Figures / Tables:

Figure 1 Figure 1: Experimental parameters, including: (a) thermodynamic calculations showing when H2 is expected to absorb and desorb from pure Pd as a function of temperature and pressure, and (b) SRIM prediction, shown for a fluence of 1017 ions/cm2, of implantation depth, damage dose, and 4He concentration for 10 keV 4Hemore » into Pd at 18.7°. Lines are meant to guide the eye in (b).« less

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    Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.