Focused ion beam for improved spatially-resolved mass spectrometry and analysis of radioactive materials for uranium isotopic analysis

Reilly, Dallas D.; Beck, Chelsie L.; Buck, Edgar C.; Cliff, John; Duffin, Andrew M.; Liezers, Martin; Springer, Kellen; Tedrow, Stephanie J.; Zimmer, Mindy M.

doi:10.1016/j.talanta.2020.120720

Cited by 22 publications

(30 citation statements)

References 31 publications

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“…Other studies showed that the isotopic heterogeneity in this sample could not be fully revealed by microscale or bulk mass spectrometry techniques. 7 Here, we compliment this recent study with additional analysis demonstrating the inability of microscale techniques to reveal the true sample heterogeneity. We show that EUV TOF mappings of the 235 U/ 238 U isotope ratio using 1 µm pixels on the same heterogenous uranium fuel pellet mentioned above does not completely reveal the uranium fuel sample's heterogeneity.…”

Section: Introductionsupporting

confidence: 54%

“…Further details on sample preparation can be found elsewhere. 7,14 16 O + isotopes over the LEU and NU samples using 1 µm pixels (i.e., sample step size) at a laser fluence of ~1 J/cm 2 with mapping field sizes of ~25 µm x 25 µm (Figure 1B,C). The same isotopes were re-mapped over a small ~20 µm x 1 µm area of the LEU sample using 100 nm pixels at a laser fluence of <1 J/cm 2 (Figure 1D), 14 laser conditions previously used to ablate craters in resist with a diameter ≤400 nm and depth ≤40 nm.…”

Section: Methodsmentioning

confidence: 99%

“…Mass spectral imaging with high spatial resolution is important in fields such as biology, 1-3 geology, 4,5 and nuclear forensics [6][7][8][9] because it enables visualization of the spatial distribution of chemical/isotopic features of interest. Standard laser-based mass spectrometry methods, such as matrix assisted laser desorption and ionization (MALDI) and laser ablation inductively coupled plasma (LA ICP) mass spectrometry, are widely used for mapping molecular (MALDI MS), elemental, and isotopic (LA ICP-MS) information but are usually limited to analyses at the micron scale.…”

Section: Introductionmentioning

confidence: 99%

“…Standard laser-based mass spectrometry methods, such as matrix assisted laser desorption and ionization (MALDI) and laser ablation inductively coupled plasma (LA ICP) mass spectrometry, are widely used for mapping molecular (MALDI MS), elemental, and isotopic (LA ICP-MS) information but are usually limited to analyses at the micron scale. 1,7,10,11 Nanoscale secondary ionization mass spectrometry (NanoSIMS), an ion sputtering and ionization method, has become the leader in elemental and isotopic analyses at the nanoscale, achieving a lateral spatial resolution of <100 nm. 3,5 Recently, we have shown that an extreme ultraviolet (EUV) laser coupled to a mass spectrometer can also offer unsurpassed three-dimensional (3D) nanoscale spatial resolution for chemical mapping.…”

Section: Introductionmentioning

confidence: 99%

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Imaging isotopic content at the nanoscale using extreme ultraviolet laser ablation and ionization mass spectrometry

Rush

Cliff

Reilly

et al. 2021

International Conference on X-Ray Lasers 2020

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Extreme ultraviolet (EUV) lasers possess unique properties for ablation and ionization at the nanoscale (≤100 nm) due to their short wavelength, high absorptivity in most materials (i.e., 10's of nanometers), and efficient photoionization in the laser-created plasmas. When coupled with a mass spectrometer, an EUV laser can be used to analyze and map chemical information in three dimensions with nanoscale spatial resolution. We have previously built an EUV time-of-flight mass spectrometer (EUV TOF) that achieved ~80 nm lateral and ~20 nm depth resolution when mapping the chemical content in organic and inorganic solids. Here, we present results from a recent study that extends EUV TOF's high resolution capabilities to the analysis of an isotopically heterogenous uranium fuel pellet that was made by blending two isotopically distinct starting materials. We show that EUV TOF can map 235 U/ 238 U heterogeneity at the 100 nm scale, revealing micron to submicron heterogeneity. For comparison, nanoscale secondary ionization mass spectrometry (NanoSIMS) maps a similar distribution of U heterogeneity on a similar subsample at the same spatial scale. We also show that EUV TOF can measure the isotope ratio in a silver sample using single shot spectra. These results position EUV TOF as a promising technique for performing isotopic analyses at the nanoscale, finding applications in nuclear forensics, geology, and biology as well as in the semiconductor industry.

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Section: Introductionsupporting

confidence: 54%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Imaging isotopic content at the nanoscale using extreme ultraviolet laser ablation and ionization mass spectrometry

Rush

Cliff

Reilly

et al. 2021

International Conference on X-Ray Lasers 2020

Self Cite

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“…Additionally, with the use of the sample preparation technique of FIB-SEM system, mass spectroscopy techniques such as thermal ionization mass spectrometry (TIMS) and quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS) could offer some level of spatial resolution that was not typically available [111]. In the future, FIB will remain an important link between different microanalytical platforms from the macroscopic to microscopic scale, which will further promote the development of analytical methods and new technologies for the advanced characterization of the Earth and planetary materials.…”

Section: Other Complementary Techniquesmentioning

confidence: 99%

Application of FIB-SEM Techniques for the Advanced Characterization of Earth and Planetary Materials

Wang

Tang

et al. 2020

Scanning

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Advanced microanalytical techniques such as high-resolution transmission electron microscopy (HRTEM), atom probe tomography (APT), and synchrotron-based scanning transmission X-ray microscopy (STXM) enable one to characterize the structure and chemical and isotopic compositions of natural materials down towards the atomic scale. Dual focused ion beam-scanning electron microscopy (FIB-SEM) is a powerful tool for site-specific sample preparation and subsequent analysis by TEM, APT, and STXM to the highest energy and spatial resolutions. FIB-SEM also works as a stand-alone technique for three-dimensional (3D) tomography. In this review, we will outline the principles and challenges when using FIB-SEM for the advanced characterization of natural materials in the Earth and Planetary Sciences. More specifically, we aim to highlight the state-of-the-art applications of FIB-SEM using examples including (a) traditional FIB ultrathin sample preparation of small particles in the study of space weathering of lunar soil grains, (b) migration of Pb isotopes in zircons by FIB-based APT, (c) coordinated synchrotron-based STXM characterization of extraterrestrial organic material in carbonaceous chondrite, and finally (d) FIB-based 3D tomography of oil shale pores by slice and view methods. Dual beam FIB-SEM is a powerful analytical platform, the scope of which, for technological development and adaptation, is vast and exciting in the field of Earth and Planetary Sciences. For example, dual beam FIB-SEM will be a vital technique for the characterization of fine-grained asteroid and lunar samples returned to the Earth in the near future.

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Role of Nuclear Forensics in Preparedness and Response in Radiation Emergencies

Maity,

Pant,

Police

et al. 2024

Handbook on Radiation Environment, Volume 1

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Focused ion beam for improved spatially-resolved mass spectrometry and analysis of radioactive materials for uranium isotopic analysis

Cited by 22 publications

References 31 publications

Imaging isotopic content at the nanoscale using extreme ultraviolet laser ablation and ionization mass spectrometry

Imaging isotopic content at the nanoscale using extreme ultraviolet laser ablation and ionization mass spectrometry

Application of FIB-SEM Techniques for the Advanced Characterization of Earth and Planetary Materials

Role of Nuclear Forensics in Preparedness and Response in Radiation Emergencies

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