Atom probe tomography

Gault, Baptiste; Chiaramonti, Ann N.; Cojocaru‐Mirédin, Oana; Stender, Patrick; Dubosq, Renelle; Freysoldt, Christoph; Makineni, Surendra Kumar; Li, Tong; Moody, Michael P.; Cairney, Julie M.

doi:10.1038/s43586-021-00047-w

Cited by 181 publications

(99 citation statements)

References 480 publications

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“…comprehensively covers APT. 68 The mass transport kinetics of oxide materials can be derived experimentally using oxygen isotope exchange depth profile technique coupled with secondary ion mass spectrometry (SIMS) 69…”

Section: Operation Measurementsmentioning

confidence: 99%

Silica: ubiquitous poison of metal oxide interfaces

et al. 2022

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Section: Operation Measurementsmentioning

confidence: 99%

Silica: ubiquitous poison of metal oxide interfaces

et al. 2022

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“…Atom probe tomography (APT) can provide 3D constructions of samples containing any element, with a sensitivity in the order of parts per millions and down to sub-nanometer resolution. [268] Jiang et al [266] demonstrate one method of sample preparation through a nanofabrication "sandwich," embedding their O 2 reduction Fe-CNT electrocatalyst between layers of Ni, Au and Si and milling a sample tip using a focused ion beam (Figure 21a). Their APT results suggest Fe atoms may directly coordinate to both C and O (Figure 21b).…”

Section: Atom Probe Tomographymentioning

confidence: 99%

“…[268] Nevertheless, looking toward the future with the advent of new sample preparation routes, laser pulsing, and detectors, APT presents a possible pathway to measuring the identity and coordination nature of dual-atoms catalytic sites as well as all surrounding atoms, thus becoming a complementary characterization to STEM (Section 4.1.1) and X-ray absorption spectroscopy (Section 4.2.1). [268] 4.2. Spectroscopy and Spectrometry…”

Section: Atom Probe Tomographymentioning

confidence: 99%

“…[ 266 ] This reveals one limitation of APT; the nanoscale sample volume analyzed results in 10 7 –10 8 ion counts, whereas time‐of‐flight secondary ion mass spectrometry (Section 4.2.4) and inductively coupled plasma mass spectrometry (Section 4.2.6) analyze µm 3 ‐mm 3 sample volumes, resulting in >10 9 ions. [ 268 ] Nevertheless, looking toward the future with the advent of new sample preparation routes, laser pulsing, and detectors, APT presents a possible pathway to measuring the identity and coordination nature of dual‐atoms catalytic sites as well as all surrounding atoms, thus becoming a complementary characterization to STEM (Section 4.1.1) and X‐ray absorption spectroscopy (Section 4.2.1). [ 268 ]…”

Section: Advanced Characterizationmentioning

confidence: 99%

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Dual‐Metal Atom Electrocatalysts: Theory, Synthesis, Characterization, and Applications

Pedersen

Barrio

et al. 2021

Advanced Energy Materials

107

106

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a required reduction in emissions per unit production of 75% by 2050 in order to have a 50% chance of limiting global mean temperature rise by 2 °C compared to pre-industrial levels. [1,2] Improvements in the field of electrocatalysts, especially in relation to electrolyzers and fuel cells, will help these devices become part of the solution to the looming sustainable energy and chemical production needs. [3] For these devices to be entirely renewable, H 2 (and O 2 ) needs to be produced by water splitting in electrolyzers through H 2 and O 2 evolution (green hydrogen production), rather than from methane reforming (grey hydrogen production). [4,5] H 2 can then be used in electrochemical O 2 reduction in fuel cells to produce electricity. [6,7] Meanwhile, electrochemical reduction of N 2 to NH 3 can provide a sustainable means to a critical fertilization source for the agricultural industry and a carrier for H 2 . [8] Moreover, a way of producing value-added products and a "circular economy" for industry from CO 2 emissions is via the electrocatalytically driven CO 2 reduction, which converts CO 2 to essential feedstocks, such as ethylene or ethanol for the chemical industry. [9] Low-temperature fuel cells and electrolyzers typically utilize catalysts based on platinum group metal (PGM) nanoparticles, [10] which limits device commercialization due to increasing global demand, low uptake of recycling, and high cost of PGMs. [11] Consequently, many researchers have turned their attention to reducing PGM loading or entirely replacing them with lower-cost earth-abundant metals, such as Fe, Cu, Ni, Co, Mn, and, most recently, Sn. [12] Regardless of the catalyst composition, improvements in the electrochemical activity have been highly sought after with two general options available; increasing the number of accessible catalytic sites and/or increasing the intrinsic activity of the catalytic sites. [13] Many different catalyst designs have been explored in order to raise the activity, such as alloying [14] or nanostructuring. [15] While increasing the density of catalytic sites improves activity, this method becomes physically limited when catalyst loading affects charge and mass transport. [13] Thus, improving the activity per catalytic site (intrinsic activity) through controlling local geometry and electronic structure has garnered research attention, with successful methods including shrinking the catalytic site down to atomic scale, as well as locally introducing light heteroatoms or hosting the catalytic site at edges. [10,[16][17][18] Electrochemical clean energy conversion and the production of sustainable chemicals are critical in the journey to realizing a truly sustainable society. To progress electrochemical storage and conversion devices to commercialization, improving the electrocatalyst performance and cost are of utmost importance. Research into dual-metal atom catalysts (DACs) is rising in prominence due to the advantages of these sites over single-metal atom catalysts (SACs), such as breaking scaling ...

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“…Atom probe tomography (APT) has the ability to detect all elements irrespective of their mass [5], and provides three-dimensional compositional mapping with sub-nanometer resolution [6]. This unique combination of high spatial resolution and chemical sensitivity is necessary to enable observations and quantification of hydrogen at specific microstructural features within complex materials.…”

Section: Introductionmentioning

confidence: 99%

Origins of the hydrogen signal in atom probe tomography: case studies of alkali and noble metals

et al. 2022

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Atom Probe Tomography (APT) analysis is being actively used to provide near-atomic-scale information on the composition of complex materials in three-dimensions. In recent years, there has been a surge of interest in the technique to investigate the distribution of hydrogen in metals. However, the presence of hydrogen in the analysis of almost all specimens from nearly all material systems has caused numerous debates as to its origins and impact on the quantitativeness of the measurement. It is often perceived that most H arises from residual gas ionization, therefore affecting primarily materials with a relatively low evaporation field. In this work, we perform systematic investigations to identify the origin of H residuals in APT experiments by combining density-functional theory (DFT) calculations and APT measurements on an alkali and a noble metal, namely Na and Pt, respectively. We report that no H residual is found in Na metal samples, but in Pt, which has a higher evaporation field, a relatively high signal of H is detected. These results contradict the hypothesis of the H signal being due to direct ionization of residual H2 without much interaction with the specimen's surface. Based on DFT, we demonstrate that alkali metals are thermodynamically less likely to be subject to H contamination under APT-operating conditions compared to transition or noble metals. These insights indicate that the detected H-signal is not only from ionization of residual gaseous H2 alone, but is strongly influenced by material-specific physical properties. The origin of H residuals is elucidated by considering different conditions encountered during APT experiments, specifically, specimen-preparation, transportation, and APT-operating conditions by taking thermodynamic and kinetic aspects into account.

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Atom probe tomography

Cited by 181 publications

References 480 publications

Silica: ubiquitous poison of metal oxide interfaces

Silica: ubiquitous poison of metal oxide interfaces

Dual‐Metal Atom Electrocatalysts: Theory, Synthesis, Characterization, and Applications

Origins of the hydrogen signal in atom probe tomography: case studies of alkali and noble metals

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