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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. doi: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 = {Thu Aug 01 00:00:00 EDT 2019},
month = {Thu Aug 01 00:00:00 EDT 2019}
}

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Cited by: 8 works
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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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Works referenced in this record:

Energetics and formation kinetics of helium bubbles in metals
journal, January 1983


Review of absorption and adsorption in the hydrogen–palladium system
journal, August 2006


Interaction of Hydrogen with Defects in Metals: Interplay between Theory and Experiment
journal, November 1982


Helium implantation effects in palladium at high doses
journal, January 1973


Low-temperature He 3 NMR studies in aged palladium tritide
journal, September 1991


Dislocation loop punching in bubble arrays
journal, January 1989


Interaction of hydrogen isotopes with metals: Deuterium trapped at lattice defects in palladium
journal, September 1990

  • Besenbacher, F.; Nielsen, B. Bech; N�rskov, J. K.
  • Journal of Fusion Energy, Vol. 9, Issue 3
  • DOI: 10.1007/BF01059239

Hydrogen interactions with defects in crystalline solids
journal, April 1992


On the correlation between mechanical and TEM studies of the aging of palladium during tritium storage
journal, June 2005


The H-Pd (hydrogen-palladium) System
journal, February 1994

  • Manchester, F. D.; San-Martin, A.; Pitre, J. M.
  • Journal of Phase Equilibria, Vol. 15, Issue 1
  • DOI: 10.1007/BF02667685

Helium bubbles in palladium tritide
journal, June 1983


Activation energy for diffusion of point defects at the surfaces of F.C.C. metals
journal, June 1997

  • Eremeev, S. V.; Lipnitskii, A. G.; Potekaev, A. I.
  • Russian Physics Journal, Vol. 40, Issue 6
  • DOI: 10.1007/BF02766393

Ion beam studies of hydrogen in metals
journal, March 1985


SRIM – The stopping and range of ions in matter (2010)
journal, June 2010

  • Ziegler, James F.; Ziegler, M. D.; Biersack, J. P.
  • Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 268, Issue 11-12
  • DOI: 10.1016/j.nimb.2010.02.091

On the use of SRIM for computing radiation damage exposure
journal, September 2013

  • Stoller, R. E.; Toloczko, M. B.; Was, G. S.
  • Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 310
  • DOI: 10.1016/j.nimb.2013.05.008

The Palladium-Hydrogen System
journal, August 1991


The pressure for dislocation loop punching by a single bubble
journal, August 1988


TEM study of the aging of palladium-based alloys during tritium storage
journal, February 2000


Transmission electron microscopy with in situ ion irradiation
journal, February 2015


The role of palladium in a hydrogen economy
journal, June 2011


Helium release and electron-microscopy of helium-implanted palladium
journal, January 1972


Solubility of hydrogen isotopes in palladium
journal, July 1983


Radiation Damage in Pd Produced by 1-3-MeV Electrons
journal, January 1967


NIH Image to ImageJ: 25 years of image analysis
journal, June 2012

  • Schneider, Caroline A.; Rasband, Wayne S.; Eliceiri, Kevin W.
  • Nature Methods, Vol. 9, Issue 7
  • DOI: 10.1038/nmeth.2089

NMR evidence for solid-fluid transition near 250 K of He 3 bubbles in palladium tritide
journal, August 1987


New Microscope and Ion Accelerators for Materials Investigations (MIAMI-2) system at the University of Huddersfield
journal, July 2019

  • Greaves, G.; Mir, A. H.; Harrison, R. W.
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 931
  • DOI: 10.1016/j.nima.2019.03.074

The palladium-hydrogen system
journal, September 1937


Drilling accurate nanopores for biosensors by energetic multi-wall carbon nanotubes: a molecular dynamics investigation
journal, September 2022


Helium bubbles in palladium tritide
journal, June 1983


Ion beam studies of hydrogen in metals
journal, March 1985


Review of absorption and adsorption in the hydrogen–palladium system
journal, August 2006


On the correlation between mechanical and TEM studies of the aging of palladium during tritium storage
journal, June 2005


Intermediate energy proton irradiation: Rapid, high-fidelity materials testing for fusion and fission energy systems
journal, February 2021


On the use of SRIM for computing radiation damage exposure
journal, September 2013

  • Stoller, R. E.; Toloczko, M. B.; Was, G. S.
  • Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 310
  • DOI: 10.1016/j.nimb.2013.05.008

Energetics and formation kinetics of helium bubbles in metals
journal, January 1983


The pressure for dislocation loop punching by a single bubble
journal, August 1988


Dislocation loop punching in bubble arrays
journal, January 1989


The Palladium-Hydrogen System
journal, August 1991


Transmission electron microscopy with in situ ion irradiation
journal, February 2015


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