As hydrogen is touted as a key player in the decarbonization of modern society, it is critical to enable quantitative hydrogen (H) analysis at high spatial resolution and, if possible, at the atomic scale. H has a known deleterious impact on the mechanical properties (strength, ductility, toughness) of most materials that can hinder their use as part of the infrastructure of a hydrogen-based economy. Enabling H mapping including local hydrogen concentration analyses at specific microstructural features is essential for understanding the multiple ways that H affect the properties of materials including embrittlement mechanisms and their synergies. In addition, spatial mapping and quantification of hydrogen isotopes is essential to accurately predict tritium inventory of future fusion power plants thus ensuring their safe and efficient operation. Atom probe tomography (APT) has the intrinsic capability to detect H and deuterium (D), and in principle the capacity for performing quantitative mapping of H within a material's microstructure. Yet, the accuracy and precision of H analysis by APT remain affected by complex field evaporation behavior and the influence of residual hydrogen from the ultrahigh vacuum chamber that can obscure the signal of H from within the material. The present article reports a summary of discussions at a focused workshop held at the Max-Planck Institute for Sustainable Materials in April 2024. The workshop was organized to pave the way to establishing best practices in reporting APT data for the analysis of H. We first summarize the key aspects of the intricacies of H analysis by APT and then propose a path for better reporting of the relevant data to support interpretation of APT-based H analysis in materials.

As part of the Avogadro constant re-determination, the molar mass of a highly-enriched Si-28 crystal is being determined using various mass-spectrometry techniques. These calculations rely on the silicon material having high chemical purity, which has been initially assessed by infrared spectrometry. APT is uniquely suited to assess isotopic purity and distribution within a sample, thus ensuring the homogeneity required for precise measurements. In this study, Atom Probe Tomography (APT) is employed to further investigate isotopic composition and elemental purity within the mono-isotopically highly-enriched Si-28 crystal (AVO28) and ultra-highly-enriched Si-28 (UHP) and contrasted with natural silicon isotopes samples (WASO04, PSM, and SRM990). Reliable silicon isotope ratios are obtained from standard samples through a data processing procedure which utilizes automated mass ranging, background and deadtime corrections. The Si-29/Si-28 isotope ratios for WASO04, PSM and SRM990 agree with published values. AVO28 and UHP analysis reveals no impurities detected above 2 mu g/g, with a uniform distribution of Si-28 and Si-29 at the nanometer scale. AVO28 exhibits Si-29 content of 41 +/- 2 mu g/g, with no detection of Si-30 below 2 mu g/g, consistent with SIMS and other international comparisons. This work demonstrates APT's capability for impurity detection and high-precision isotope analysis, reinforcing the silicon molar mass calculations and supporting Avogadro's constant redefinition.

Journal Article Improving Analytical Capability via Simultaneous Voltage and Laser Pulsing in Atom Probe Tomography Get access David J Larson, David J Larson CAMECA Instruments Inc., Madison WI, USA Corresponding author: David.larson@ametek.com Search for other works by this author on: Oxford Academic Google Scholar Ty J Prosa, Ty J Prosa CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Yimeng Chen, Yimeng Chen CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar David A Reinhard, David A Reinhard CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Isabelle Martin, Isabelle Martin CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Robert M Ulfig, Robert M Ulfig CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Michael Holman, Michael Holman CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Jesse Robinson, Jesse Robinson CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Dan Lenz Dan Lenz CAMECA Instruments Inc., Madison WI, USA Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 29, Issue Supplement_1, 1 August 2023, Pages 609–610, https://doi.org/10.1093/micmic/ozad067.295 Published: 22 July 2023

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Journal Article Site-Specific Lift-Out on Complicated Nanoscale Structures Get access Yimeng Chen, Yimeng Chen CAMECA Instruments Inc., Madison, WI 53711 USA Corresponding author: Yimeng.Chen@ametek.com Search for other works by this author on: Oxford Academic Google Scholar Ty J Prosa Ty J Prosa CAMECA Instruments Inc., Madison, WI 53711 USA Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 92–93, https://doi.org/10.1017/S1431927622001271 Published: 01 August 2022

The segregation of reactive elements (REs) along thermally grown oxide (TGO) grain boundaries has been associated to slower oxide growth kinetics and improved creep properties. However, the incorporation and diffusion of these elements into the TGO during oxidation of Ni alloys remains an open question. In this work, electron backscatter diffraction in transmission mode (t-EBSD) was used to investigate the microstructure of TGO within the thermal barrier coating on a Ni-based superalloy, and atom probe tomography (APT) was used to quantify the segregation behavior of REs to α-Al2O3 grain boundaries. Integrating the two techniques enables a higher level of site-specific analysis compared to the routine focused ion beam lift-out sample preparation method without t-EBSD. Needle-shaped APT specimens readily meet the thickness criterion for electron diffraction analysis. Transmission EBSD provides an immediate feedback on grain orientation and grain boundary location within the APT specimens to help target grain boundaries in the TGO. Segregation behavior of REs is discussed in terms of the grain boundary character and relative location in TGO.

The interaction between laser-pulsed radiation and APT specimens can be complex [1,2], but from a microscopy perspective, the key considerations really only depend on the microscopy outcomes: time-to-knowledge and information content of the characterization. Commercially available atom probes have provided infrared, green, blue, and ultra-violet (UV) options for laser-pulsed acquisition, with the LEAP ® 4000/5000 platforms utilizing 355-nm light. The newest atom probes, the LEAP 6000 and Invizo™ 6000, utilize deep-ultra-violet (DUV) 266-nm light [3]. Published studies investigating the correlations between acquisition parameters and survivability have been rather limited In a previous study, we focused on the survivability of a silicon sample containing a 12-nm silicon-oxide layer as a good indicator of general trade-offs between variables like detection rate (DR), pulse frequency, and laser pulse energy (LPE) for survivability We showed that the total rate of atom removal (DR and pulse frequency) was the key variable, while the LPE energy and its role in reducing the evaporation field was also important, but secondary. Although not an aim of the study, the fastest acquisition rates which provided high (>80%) survivability were performed at 0.4% DR and 625 kHz at 355-nm (the only wavelength evaluated in that study). In this presentation, we report on progress evaluating a similar analysis space of this same sample using DUV and the automated features available on the 6000 atom probe platforms as an on-going study. As of the writing of this abstract, we have collected some

Atom probe tomography (APT) has been an important technique for metallurgical research for more than 50 years, but only recently has there been substantial adoption in the semiconductor industry [1–3]. Maintaining this trend requires continuing advances in the areas of hardware (and software) related to APT. The field-of-view (FOV) / mass-spectral-quality tradeoff [4] along with laser wavelength [5,6] are two such areas of advancement. It is highly desirable for an atom probe to have a combination of a wide field of view and high mass resolving power (MRP), but historically, these two metrics are inherently at odds with each other, from a design perspective. Some efforts to overcome this difficulty employ reflectron energy compensating based solutions [7], while others use a straight flight path design [8,9]. In this work, we present the new CAMECA Invizo 6000 TM atom probe and introduce the primary benefits.

Journal Article A Reconstruction Wizard for Electrostatic Reconstruction Get access Brian P Geiser, Brian P Geiser CAMECA Instruments Inc, Fitchburg, WI, USA Corresponding author: Brian.Geiser@ametek.com Search for other works by this author on: Oxford Academic Google Scholar David Reinhard, David Reinhard CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Joseph Bunton, Joseph Bunton CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar David Larson, David Larson CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Robert Ulfig, Robert Ulfig CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Katherine P Rice, Katherine P Rice CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Isabelle Martin, Isabelle Martin CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Yimeng Chen, Yimeng Chen CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Ty Prosa, Ty Prosa CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Tim Payne Tim Payne CAMECA Instruments Inc, Fitchburg, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 704–705, https://doi.org/10.1017/S1431927622003282 Published: 01 August 2022

Journal Article New Product Announcement – LEAP 6000XR, New Applications, New Performance Get access Robert Ulfig, Robert Ulfig CAMECA Instruments Inc., Madison, WI, USA Corresponding author: Robert.Ulfig@AMETEK.com Search for other works by this author on: Oxford Academic Google Scholar Daniel Lenz, Daniel Lenz CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Gard Groth, Gard Groth CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Joseph H Bunton, Joseph H Bunton CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Isabel Martin, Isabel Martin CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Ty J Prosa, Ty J Prosa CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar David A Reinhard, David A Reinhard CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Peter H Clifton, Peter H Clifton CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Brian P Geiser, Brian P Geiser CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar David J Larson David J Larson CAMECA Instruments Inc., Madison, WI, USA Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 3190–3191, https://doi.org/10.1017/S1431927622011849 Published: 01 August 2022

Atom probe tomography (APT) is a technique that has expanded significantly in terms of adoption, dataset size, and quality during the past 15 years. The sophistication used to ensure ultimate analysis precision has not kept pace. The earliest APT datasets were small enough that deadtime and background considerations for processing mass spectrum peaks were secondary. Today, datasets can reach beyond a billion atoms so that high precision data processing procedures and corrections need to be considered to attain reliable accuracy at the parts-per-million level. This paper considers options for mass spectrum ranging, deadtime corrections, and error propagation as applied to an extrinsic-silicon standard specimen to attain agreement for silicon isotopic fraction measurements across multiple instruments, instrument types, and acquisition conditions. Precision consistent with those predicted by counting statistics is attained showing agreement in silicon isotope fraction measurements across multiple instruments, instrument platforms, and analysis conditions.

Atom probe tomography (APT) has been incorporated into a wide variety of materials research applications over the course of the past twenty years as the installed base of atom probes has increased from single digits to over one hundred [1]. Despite this increase, and the corresponding technology advances, there are still challenges to further adoption. This abstract discusses some of the key challenges of yield and reconstruction and some of the avenues CAMECA ® is exploring to overcome them. A primary may

Li ion batteries are widely used for portable PCs, cellular phones and other portable electronics. A recent market forecast predicts a massive expansion in production driven by electric vehicles. An anode, a cathode and an electrolyte are the three main components in a Li-ion battery. Most cathode materials are made of a Li-based oxide to provide mobile Li ions. Lithium-cobalt-oxide comprised over 34% of the market share in 2018; however, lithium-nickel-manganese-cobalt (NMC) [1]. Its market share is expected to increase to 48% in 2025 from the current 19%. The shift is already taking place by major manufactures owing to its in addition to cost competitiveness. NMC shows high capacity and power flow of 150-220 Wh/kg, a nominal voltage of 3.6V and a 1000-2000 cycle life [1]. Manufacturing R&D also shows a trend of shifting to high Ni content systems for enhanced capacity. In this work we investigate the composition and fine-scale microstructure analysis of two types of NMC cathode materials. Cathode tapes with 90% active particle, 5% binder and 5% conductive carbon were obtained from NEI Corporation (product names EB-50E-622 and EB-50E-811). The nominal compositions are Li(NixMnyCoz)O2 X:Y:Z=6:2:2 and X:Y:Z=8:1:1. SEM and EDS analysis on these materials confirms the particles are ~10 um in diameter and compositionally homogeneous at the sub-micron scale. Standard atom probe tomography specimen preparation method with focused ion beam lift-out was used for analysis of the sub surface region

An abstract is not available for this content so a preview has been provided. As you have access to this content, a full PDF is available via the ‘Save PDF’ action button.

An abstract is not available for this content so a preview has been provided. As you have access to this content, a full PDF is available via the 'Save PDF' action button.

In atom probe tomography (APT) a primary element of the instrument optics is the specimen itself. In order to correct artifacts in the data caused by an evolving apex shape, we are developing a numerical electrostatic model [1, 2] reflecting the physics of both the instrumental pieces as well as the specimen geometry. In this poster we report on some numerical accuracy metrics of this model and illustrate its use in the generation of simulated evaporation data.

The design of multiphase optical nanocomposites necessitates the understanding of coexisting phases’ morphology and chemistry which have deterministic impacts on light–matter interaction. A prominent example is gradient refractive index (GRIN) materials proposed to realize an arbitrarily shaped, single optical component with minimal chromatic aberration. Ge‐As‐Pb‐Se materials are promising for GRIN due to their ability to exhibit spatially varying volume fraction of high‐index Pb‐rich phases in low index matrices. These materials are characterized to date, exclusively using transmission electron microscopy to reveal their phase separation and induced crystalline phase(s). It is found in the study that the intrinsic 2D perspective of the technique has hindered the identification of true morphology. To clarify this ambiguity, atom probe tomography (APT) is utilized to gain the first‐ever observation of the nanocomposites’ microstructure and its evolution upon heat treatment in a 3D space. The APT‐quantified geometry and chemistry of coexisting phases are considered to predict the effective media's optical behaviors which closely match experimental data, enabling the establishment of the material's predictive and accurate process–structure–property relationship. Findings in the study demonstrate the robustness and advantage of the APT‐assisted characterization in the design and realization of GRIN materials.

An advanced technique for site-specific Atom Probe Tomography (APT) is presented. An APT sample is prepared from a targeted semiconductor device (commercially available product based on 14nm finFET technology). Using orthogonal views of the sample in STEM while FIB milling, a viable APT sample is created with the tip of the sample positioned over the lightly-doped drain (LDD) region of a pre-defined PFET. The resulting APT sample has optimal geometry and minimal amorphization damage.

In atom probe tomography, a multi-hit event is defined as more than one ion detected during a single laser or voltage pulse. The multiplicity is the number of recorded ions for a single pulse. For some materials and analysis conditions, multi-hit events may be present in as many as 60% of recorded pulses. Common examples of applications with high multiplicity are oxides, III/V compounds, carbon in steels and both boron and carbon in silicon [1]. In general, the compounds made of ionic or covalent bonding are known to produce multi-hit events at much higher rates than predicted by random (uncorrelated) evaporations. Ion dissociation and post-ionization are the main factors that are thought to contribute to high multiplicity events. Non-random (correlated) evaporations can result in non-detectable ions (e.g. may not even appear as multi-hit events) that can bias compositional measurement. In some cases, accurate compositional measurements cannot be made without correction factors.