Analysis of zirconium–niobium pressure tube surfaces for hydrogen using secondary ion mass spectrometry (SIMS)

McIntyre, N. S.; Weisener, Christopher G.; Davidson, R. D.; Lennard, W. N.; Massoumi, G.R.; Mitchell, I.V.; Brennenstuhl, A.M.; Warr, BD

doi:10.1002/sia.740151004

Cited by 15 publications

(8 citation statements)

References 12 publications

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“…The SIMS technique has been widely utilized to investigate the surface and depth distribution analysis of hydrogen and deuterium in various matrices. [11][12][13][14][15][16] For instance, Stevie has utilized the technique for determining the concentration depth profile of hydrogen in ionimplanted silicon and niobium samples. 11 The samples were selected based on the hydrogen mobility criteria.…”

Section: Previous Studies-sims Analysis Of Hydrogen and Deuterium In ...mentioning

confidence: 99%

“…SIMS technique has also been widely utilized for determining the 2 H concentration in various nuclear materials. For example, McIntyre et al studied the capabilities of SIMS and NRA for quantification of 1 H and 2 H in Zr2.5Nb irradiated pressure tubes 14 . They concluded that the shape and peak of 2 H in 2 H‐implanted Zr2.5Nb samples have been altered due to the outward and inward migration of 2 H in Zr2.5Nb.…”

Section: Introductionmentioning

confidence: 99%

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Determination of relative sensitivity factor, sputtering rate, and detection limits of deuterium in deuterium ion‐implanted Zircaloy‐4 using secondary ion mass spectrometer

Singh

Karki

Jaison

2022

Surface & Interface Analysis

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Zirconium‐based alloys are extensively used in the nuclear industry as materials for reactor core components. These alloys are used in fuel cladding and pressure tubes with 1H2O or 2H2O as the primary heat exchange fluid. Continuous usage of pressure tubes and fuel cladding inside the reactor results in heavy ingress of hydrogen (1H) or deuterium (2H), which gives rise to the formation of hydrogen (or deuterium) precipitates in the host of zirconium matrix. This is called hydrogen (or deuterium) embrittlement phenomenon. Therefore, determination of hydrogen or deuterium concentration periodically in zirconium alloy pressure tubes and cladding are crucial for safe operation of nuclear reactors. Hence, in this work, secondary ion mass spectrometry (SIMS) has been utilized to determine the relative sensitive factor (RSF), sputtering rate, and detection limits of 2H in 2H+ ion‐implanted Zircaloy‐4 sample. SIMS analysis has been carried out using O2+ and Cs+ primary ion beams. Depth profiles of various elemental and molecular secondary ions have been monitored to determine the RSF values and detection limits of 2H in the sample under different primary ion beam analysis conditions. Sputtering rate under different analysis conditions has also been determined from the correlation between the projected range of 2H+ ions in Zircaloy‐4 sample determined from Stopping and Range of Ions in Matter (SRIM) software and the depth of the crater formed by primary ion beam bombardment process. The projected range of 2H+ ions in Zircaloy‐4 was estimated to be ~524.2 nm using the simulation carried out by SRIM software. The projected range, evaluated by SRIM software, was utilized for depth scale calibration of SIMS sputtered time profiles. The SIMS depth profiles were also calibrated by determining the depth of the SIMS crater by using optical depth profilometer. The values of range estimated by SRIM as well as optical profilometer were found to be in good agreement, within instrument uncertainty.

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Section: Previous Studies-sims Analysis Of Hydrogen and Deuterium In ...mentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Determination of relative sensitivity factor, sputtering rate, and detection limits of deuterium in deuterium ion‐implanted Zircaloy‐4 using secondary ion mass spectrometer

Singh

Karki

Jaison

2022

Surface & Interface Analysis

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“…An example of the effect of hydrogen mobility was provided by SIMS analysis of ZrNb. Depth profiles of deuterium implanted into ZrO 2 on a ZrNb alloy substrate were compared with analyses on the same implant into the substrate . The implant was at 40 keV to a dose of 1 × 10 16 atoms/cm 2 .…”

Section: Samples and Techniquesmentioning

confidence: 99%

Analysis of hydrogen in materials with and without high hydrogen mobility

Stevie

2016

Surface & Interface Analysis

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Hydrogen is a very important element but analysis of hydrogen in solids can be difficult and is not available for many analytical techniques. This paper provides an overview of the capabilities of SIMS and NRA to measure hydrogen concentrations and distributions. Bulk analysis methods provide an overall result, but depth profiles are often needed. SIMS can produce useful and quantifiable depth profiles for hydrogen and the isotopes deuterium and tritium. Hydrogen analysis at the surface and imaging with good lateral resolution can also be achieved with SIMS. However, hydrogen can have high mobility in a variety of materials and this will affect SIMS analysis. For those cases, other surface analysis methods such as hydrogen forward scattering and nuclear reaction analysis are preferred. Hydrogen analysis examples in silicon and in niobium are used for materials without and with high hydrogen mobility respectively. Copyright © 2016 John Wiley & Sons, Ltd.

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“…There are several previous reports of the value of depth profiling and 3D characterization of zirconium alloys for nuclear applications by SIMS. For example the study of hydrogen or deuterium diffusion through oxides on Zr alloys, 11,7,12,13 the incorporation of cations like Li Na and K into zirconium oxide 14 and the study of second phase particles (SPPs) 15–17 . Recently, we have shown that high‐resolution SIMS analysis of oxidised zirconium alloys using a CAMECA NanoSIMS 50 instrument enables the 3D characterisation of deuterium distributions 9,18 …”

Section: Introductionmentioning

confidence: 99%

Site‐specific specimen preparation for SIMS analysis of radioactive samples

Liu

Lozano-Pérez

et al. 2020

Journal of Microscopy

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Secondary Ion Mass Spectrometry is an important technique for the study of the composition of a wide range of materials because of the exceptionally high sensitivity that allows the study of trace elements and the ability to distinguish isotopes that can be used as markers for reactions and transport processes. However, when studying nuclear materials, it is often necessary to analyse highly radioactive samples, and only rather few SIMS facilities are available in active environments. In this paper, we present a methodology using focussed ion beam milling to prepare samples from radioactive specimens that are sufficiently large to undertake SIMS mapping experiments over microstructurally significant regions, but with overall activities small enough to be readily transported and analysed by a SIMS instrument in a normal laboratory environment. Radioactive samples prepared using this methodology can also be used for correlative SIMS analysis with other analytical microscopies. SIMS results showing the distributions of deuterium in oxides on in‐reactor corroded zirconium alloys are presented to demonstrate the potential of this sample preparation technique.

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Analysis of zirconium–niobium pressure tube surfaces for hydrogen using secondary ion mass spectrometry (SIMS)

Cited by 15 publications

References 12 publications

Determination of relative sensitivity factor, sputtering rate, and detection limits of deuterium in deuterium ion‐implanted Zircaloy‐4 using secondary ion mass spectrometer

Determination of relative sensitivity factor, sputtering rate, and detection limits of deuterium in deuterium ion‐implanted Zircaloy‐4 using secondary ion mass spectrometer

Analysis of hydrogen in materials with and without high hydrogen mobility

Site‐specific specimen preparation for SIMS analysis of radioactive samples

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