ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten

Gabriel D. Parker; Tobias K. Misicko; Tanguy Teriler; Yang Xiao; Xiao Ying Yu

doi:10.1016/j.rsurfi.2025.100577

ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten

Gabriel D. Parker
, Tobias K. Misicko
, Tanguy Teriler
, Yang Xiao
, Xiao Ying Yu

Advanced Nuclear Materials

Research output: Contribution to journal › Article › peer-review

Abstract

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi₃⁺ primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.

Original language	English
Article number	100577
Journal	Results in Surfaces and Interfaces
Volume	20
DOIs	https://doi.org/10.1016/j.rsurfi.2025.100577
State	Published - Aug 2025

Funding

Gabriel D. Parker was funded by the Department of Energy SCGSR fellowship program and GRO internship program at the Oak Ridge National Laboratory (ORNL). Tobias K. Misicko was funded by the U.S. National Science Foundation (NSF) Experimental Program to Stimulate Competitive Research (EPSCoR) Louisiana grant fellowship to perform a summer internship at the Oak Ridge National Laboratory. Dr. Xiao-Ying Yu is indebted to the support of the United States (US) Department of Energy (DOE) Fusion Materials Program under the Fusion Energy Sciences Office at ORNL. The authors thank Dr. Yan-Ru Lin of ORNL for preparing the SEM-FIB liftout samples of the irradiated tungsten. This work was in part supported by the Louisiana EPSCoR, funded by the NSF under award number OIA-1946231 and the Board of Regents Support Fund. Tobias Misicko and Yang Xiao additionally appreciate the financial support from NSF's CBET division for the Engineering Research Initiation (ERI) award under grant number CBET-2347475 and the start-up fund from the College of Engineering and Science of Louisiana Tech University. ToF-SIMS analysis of the single crystal tungsten was performed using the Center for Nanophase Materials Sciences (CNMS) user proposal (CNMS2024-B-02747). ToF-SIMS analysis of the irradiated single crystal tungsten was performed in the Shared Equipment Authority (SEA) facility of the Rice University. This manuscript has been authored by UT-Battelle, LLC under Contract No. DE-AC05-00OR22725 with the U.S. DOE. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. The DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan (http://energy.gov/downloads/doe-public-access-plan). This manuscript has been authored by UT-Battelle, LLC under Contract No. DE-AC05-00OR22725 with the U.S. DOE. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. The DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan ( http://energy.gov/downloads/doe-public-access-plan ). Gabriel D. Parker was funded by the Department of Energy SCGSR fellowship program and GRO internship program at the Oak Ridge National Laboratory ( ORNL ). Tobias K. Misicko was funded by the U.S. National Science Foundation ( NSF ) Experimental Program to Stimulate Competitive Research ( EPSCoR ) Louisiana grant fellowship to perform a summer internship at the Oak Ridge National Laboratory . Dr. Xiao-Ying Yu is indebted to the support of the United States ( US ) Department of Energy ( DOE ) Fusion Materials Program under the Fusion Energy Sciences Office at ORNL . The authors thank Dr. Yan-Ru Lin of ORNL for preparing the SEM-FIB liftout samples of the irradiated tungsten. This work was in part supported by the Louisiana EPSCoR , funded by the NSF under award number OIA-1946231 and the Board of Regents Support Fund. Tobias Misicko and Yang Xiao additionally appreciate the financial support from NSF's CBET division for the Engineering Research Initiation ( ERI ) award under grant number CBET-2347475 and the start-up fund from the College of Engineering and Science of Louisiana Tech University . ToF-SIMS analysis of the single crystal tungsten was performed using the Center for Nanophase Materials Sciences (CNMS) user proposal (CNMS2024-B-02747). ToF-SIMS analysis of the irradiated single crystal tungsten was performed in the Shared Equipment Authority (SEA) facility of the Rice University.

Keywords

Isotopic composition
Neutron irradiation
Single crystal tungsten
Time-of-flight secondary ion mass spectrometry
Transmutation

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10.1016/j.rsurfi.2025.100577

Cite this

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title = "ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten",

abstract = "Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi3+ primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.",

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T1 - ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten

AU - Parker, Gabriel D.

AU - Misicko, Tobias K.

AU - Teriler, Tanguy

AU - Xiao, Yang

AU - Yu, Xiao Ying

PY - 2025/8

Y1 - 2025/8

N2 - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi3+ primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.

AB - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi3+ primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.

KW - Isotopic composition

KW - Neutron irradiation

KW - Single crystal tungsten

KW - Time-of-flight secondary ion mass spectrometry

KW - Transmutation

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DO - 10.1016/j.rsurfi.2025.100577

M3 - Article

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SN - 2666-8459

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JO - Results in Surfaces and Interfaces

JF - Results in Surfaces and Interfaces

M1 - 100577

ER -

ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten

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Keywords

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